CN112409303A - Purification method of D-pantoic acid lactone - Google Patents
Purification method of D-pantoic acid lactone Download PDFInfo
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- CN112409303A CN112409303A CN202011429206.8A CN202011429206A CN112409303A CN 112409303 A CN112409303 A CN 112409303A CN 202011429206 A CN202011429206 A CN 202011429206A CN 112409303 A CN112409303 A CN 112409303A
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- ethyl acetate
- pantoic acid
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- 238000000034 method Methods 0.000 title claims abstract description 27
- -1 D-pantoic acid lactone Chemical class 0.000 title claims abstract description 26
- 238000000746 purification Methods 0.000 title description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 93
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- SERHXTVXHNVDKA-BYPYZUCNSA-N (R)-pantolactone Chemical compound CC1(C)COC(=O)[C@@H]1O SERHXTVXHNVDKA-BYPYZUCNSA-N 0.000 claims abstract description 20
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 12
- 230000008025 crystallization Effects 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 238000007363 ring formation reaction Methods 0.000 claims description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 16
- 239000012295 chemical reaction liquid Substances 0.000 claims description 13
- OTOIIPJYVQJATP-BYPYZUCNSA-N (R)-pantoic acid Chemical compound OCC(C)(C)[C@@H](O)C(O)=O OTOIIPJYVQJATP-BYPYZUCNSA-N 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 2
- 239000012535 impurity Substances 0.000 abstract description 4
- 239000000049 pigment Substances 0.000 abstract description 4
- 239000012141 concentrate Substances 0.000 abstract description 3
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000012074 organic phase Substances 0.000 description 23
- 239000000243 solution Substances 0.000 description 23
- 239000008346 aqueous phase Substances 0.000 description 8
- GHOKWGTUZJEAQD-UHFFFAOYSA-N Chick antidermatitis factor Natural products OCC(C)(C)C(O)C(=O)NCCC(O)=O GHOKWGTUZJEAQD-UHFFFAOYSA-N 0.000 description 5
- GHOKWGTUZJEAQD-ZETCQYMHSA-N (D)-(+)-Pantothenic acid Chemical compound OCC(C)(C)[C@@H](O)C(=O)NCCC(O)=O GHOKWGTUZJEAQD-ZETCQYMHSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000006188 syrup Substances 0.000 description 4
- 235000020357 syrup Nutrition 0.000 description 4
- FAPWYRCQGJNNSJ-UBKPKTQASA-L calcium D-pantothenic acid Chemical compound [Ca+2].OCC(C)(C)[C@@H](O)C(=O)NCCC([O-])=O.OCC(C)(C)[C@@H](O)C(=O)NCCC([O-])=O FAPWYRCQGJNNSJ-UBKPKTQASA-L 0.000 description 3
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 239000012043 crude product Substances 0.000 description 2
- 238000007273 lactonization reaction Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000011713 pantothenic acid Substances 0.000 description 2
- 235000019161 pantothenic acid Nutrition 0.000 description 2
- 229940055726 pantothenic acid Drugs 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000011703 D-panthenol Substances 0.000 description 1
- 235000004866 D-panthenol Nutrition 0.000 description 1
- SNPLKNRPJHDVJA-ZETCQYMHSA-N D-panthenol Chemical compound OCC(C)(C)[C@@H](O)C(=O)NCCCO SNPLKNRPJHDVJA-ZETCQYMHSA-N 0.000 description 1
- 229930003270 Vitamin B Natural products 0.000 description 1
- 229930003571 Vitamin B5 Natural products 0.000 description 1
- 229960002079 calcium pantothenate Drugs 0.000 description 1
- 229960003949 dexpanthenol Drugs 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000001640 fractional crystallisation Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- GQTHJBOWLPZUOI-FJXQXJEOSA-M sodium D-pantothenate Chemical compound [Na+].OCC(C)(C)[C@@H](O)C(=O)NCCC([O-])=O GQTHJBOWLPZUOI-FJXQXJEOSA-M 0.000 description 1
- 235000019188 sodium D-pantothenate Nutrition 0.000 description 1
- 239000011756 sodium D-pantothenate Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000011720 vitamin B Substances 0.000 description 1
- 235000019156 vitamin B Nutrition 0.000 description 1
- 239000011675 vitamin B5 Substances 0.000 description 1
- 235000009492 vitamin B5 Nutrition 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/26—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member
- C07D307/30—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/32—Oxygen atoms
- C07D307/33—Oxygen atoms in position 2, the oxygen atom being in its keto or unsubstituted enol form
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/07—Optical isomers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
本发明公开一种D‑泛解酸内酯的提纯方法，包括以下步骤：S1、使用乙酸乙酯对D‑泛解酸的环合反应液进行萃取；S2、萃取结束后，使用活性炭对萃取液进行脱色，得到脱色液；S3、使用去离子水洗涤脱色液；S4、浓缩脱色液回收乙酸乙酯，去除水分，得到浓缩液；S5、使用乙酸乙酯溶解浓缩液；S6、蒸发结晶得到D‑泛解酸内酯湿粉。采用水洗乙酸乙酯相和蒸发结晶的方式制备D‑泛解酸内酯，不但水洗去除了水溶性杂质、色素、无机盐，结晶去除了脂溶性杂质和色素，而且蒸发结晶前浓缩去除了水分，具有产品外观均一，质量好，收率高，操作简单等特点。The invention discloses a method for purifying D-pantoic acid lactone. The liquid is decolorized to obtain a decolorized solution; S3, use deionized water to wash the decolorized solution; S4, concentrate the decolorized solution to reclaim ethyl acetate, remove water, and obtain a concentrated solution; S5, use ethyl acetate to dissolve the concentrated solution; S6, evaporative crystallization obtains D-pantolactone wet powder. D-pantolactone was prepared by washing the ethyl acetate phase with water and evaporating crystallization. Not only water-soluble impurities, pigments and inorganic salts were removed by water washing, fat-soluble impurities and pigments were removed by crystallization, but also water was removed by concentration before evaporative crystallization. , It has the characteristics of uniform appearance, good quality, high yield and simple operation.
Description
Technical Field
The invention relates to the technical field of medicinal chemistry, in particular to a method for purifying D-pantolactone.
Background
Pantothenic acid, also known as vitamin B5, is one of the water-soluble vitamin B group and is widely applied to the fields of medicines, foods, feeds, daily chemicals and the like. Pantothenic acid has two forms of D and L in nature, but only the D form has physiological activity. Because of the poor stability of D-pantothenic acid, calcium D-pantothenate, sodium D-pantothenate, D-panthenol, and the like are generally used as commercial forms thereof.
D-pantoic acid lactone is a key chiral intermediate for synthesizing D-calcium pantothenate. At present, the selective asymmetric hydrolysis of D-pantoic acid lactone in DL-pantoic acid lactone by microorganisms to obtain D-pantoic acid is widely adopted in industry, and then the lactonization of the D-pantoic acid is carried out to obtain the D-pantoic acid lactone (see US Patent 5275949, 1994).
Researches on a purification method of D-pantolactone mainly comprise aqueous solution crystallization and cooling crystallization. A method for crystallizing an aqueous solution of D-pantoic acid lactone (publication No. CN 110734415A) is disclosed, wherein when the aqueous solution is crystallized, inorganic salt is contained in the solution, and when the aqueous solution is cooled and crystallized, the inorganic salt is separated out, and a mother solution (containing a large amount of inorganic salt) is wrapped in a product, so that the D-pantoic acid lactone has low quality, such as low melting point and high ignition residue, and can not meet the requirements of downstream customers on the product quality; for the preparation of D-pantolactone by cooling crystallization, the patent of "a refining method of D-pantolactone" (publication No. CN 110862362A) mentions fractional crystallization, the obtained product has non-uniform quality, and at the same time, the method is only used for the purification of crude product and has high requirement on the quality of the crude product, and the method has poor universality. The research on the preparation of D-pantolactone by extracting D-pantolactone from the D-pantolactone cyclization reaction liquid and simultaneously evaporating and crystallizing is not mentioned.
Disclosure of Invention
The invention aims to provide a method for purifying D-pantoic acid lactone, which is preferably suitable for a solution obtained by lactonization of D-pantoic acid obtained by chiral resolution, and improves the quality and yield of the D-pantoic acid lactone.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for purifying D-pantoic acid lactone, comprising the following steps:
s1, extracting the cyclization reaction liquid of the D-pantoic acid by using ethyl acetate;
s2, after extraction is finished, decoloring the extraction liquid by using activated carbon to obtain a decolored liquid;
s3, washing the destaining solution by using deionized water;
s4, recovering ethyl acetate from the concentrated decolorized solution, and removing water to obtain a concentrated solution;
s5, dissolving the concentrated solution by using ethyl acetate;
s6, evaporating and crystallizing to obtain D-pantolactone wet powder;
s7, drying the D-pantoic acid lactone wet powder under the vacuum condition to obtain the D-pantoic acid lactone with the purity of more than or equal to 99 percent.
Further, the volume ratio of the ethyl acetate to the cyclization reaction liquid in the step S1 is 4: 1-2: 1; extracting with ethyl acetate for 3 times, mixing the organic phases after the first 2 times of extraction, standing, separating out the water phase, mixing the water phases, extracting for the third time, mechanically using the organic phases, and treating the water phase as wastewater after recovering ethyl acetate.
Further, the dosage of the activated carbon in the step S2 is 1-4% of the volume of the cyclization reaction liquid.
Further, in the step S3, the volume ratio of the deionized water to the cyclization reaction liquid is 0.5: 1-1.5: 1, and the water washing jacket is used for extracting the cyclization reaction liquid.
Further, in the step S4, the concentration temperature is 20-70 ℃, and the vacuum degree is more than or equal to 0.09 Mpa.
Further, step S4 is to control the temperature to 30-40 ℃ under vacuum condition to concentrate the organic phase and recycle ethyl acetate, and then to raise the temperature to 60-70 ℃ to concentrate and remove water.
Further, in the step S5, the water content of ethyl acetate is less than or equal to 0.2%, and the volume ratio of ethyl acetate to the cyclization reaction liquid is 0.5: 1-2: 1.
Further, in the step S6, the evaporation crystallization temperature is 20-30 ℃, and the vacuum degree is more than or equal to 0.09 Mpa.
Further, the drying temperature of the step S7 is 45-50 ℃.
The method has the advantages that the D-pantoic acid lactone is prepared by adopting the modes of washing the ethyl acetate phase with water and evaporating crystallization, so that water-soluble impurities, pigments and inorganic salts are removed by washing with water, fat-soluble impurities and pigments are removed by crystallization, and moisture is removed by concentration before evaporating crystallization, and the method has the characteristics of uniform product appearance, good quality, high yield, simple operation and the like.
Detailed Description
Example one
The invention provides a method for purifying D-pantoic acid lactone, which comprises the following steps:
s1, taking 200mL of D-pantoic acid cyclization reaction liquid, controlling the temperature to be 25-35 ℃, extracting for 10-15 min by using 200mL of ethyl acetate each time, standing for 25-30 min, separating out an organic phase, extracting for 3 times, combining the organic phases extracted for the first 2 times, standing, separating out an aqueous phase, combining the aqueous phases, extracting for the third time, and using the organic phase extracted for the third time;
s2, controlling the temperature to be 20-30 ℃, decoloring the organic phase with 4g of activated carbon for 45-60 min, and filtering to obtain a decolored solution;
s3, controlling the temperature to be 30-35 ℃, washing for 10-15 min by using 0.25 time of deionized water, standing for 25-30 min, separating out an organic phase, and repeatedly washing for 2 times;
s4, controlling the temperature to be 30-40 ℃, enabling the vacuum degree to be more than or equal to 0.09Mpa, concentrating and recovering ethyl acetate, then heating to 60-70 ℃, and concentrating and removing water to obtain a concentrated solution;
s5, adding ethyl acetate with the volume 0.5 times that of the cyclization reaction solution to dissolve the concentrated solution;
s6, controlling the temperature to be 20-25 ℃, and concentrating in vacuum to be in a syrup state; after the concentration is finished, discharging and centrifuging to obtain D-pantolactone wet powder;
s7, vacuum degree > 0.09Mpa, vacuum drying at 45-50 deg.C to obtain 109.2g (water content < 0.5%), yield 92%, purity 98.4%, and specific rotation degree 48.7 deg.
Example two
The invention provides a method for purifying D-pantoic acid lactone, which comprises the following steps:
s1, taking 200mL of D-pantoic acid cyclization reaction liquid, controlling the temperature to be 25-35 ℃, extracting for 10-15 min by using 200mL of ethyl acetate each time, standing for 25-30 min, separating out an organic phase, extracting for 3 times, combining the organic phases extracted for the first 2 times, standing, separating out an aqueous phase, combining the aqueous phases, extracting for the third time, and using the organic phase extracted for the third time;
s2, controlling the temperature to be 20-30 ℃, decoloring the organic phase with 4g of activated carbon for 45-60 min, and filtering to obtain a decolored solution;
s3, controlling the temperature to be 30-35 ℃, washing for 10-15 min by using 0.5 time of deionized water, standing for 25-30 min, separating out an organic phase, and repeatedly washing for 3 times;
s4, controlling the temperature to be 30-40 ℃, enabling the vacuum degree to be more than or equal to 0.09Mpa, concentrating and recovering ethyl acetate, then heating to 60-70 ℃, and concentrating and removing water to obtain a concentrated solution;
s5, adding ethyl acetate with the volume 0.5 times that of the cyclization reaction solution to dissolve the concentrated solution;
s6, controlling the temperature to be 20-25 ℃, and concentrating in vacuum to be in a syrup state; after the concentration is finished, discharging and centrifuging to obtain D-pantolactone wet powder;
s7, vacuum degree > 0.09Mpa, vacuum drying at 45-50 deg.C to obtain 102g (water content < 0.5%), yield 85%, purity 98.9%, and specific rotation degree 50.1 deg.C.
EXAMPLE III
The invention provides a method for purifying D-pantoic acid lactone, which comprises the following steps:
s1, taking 200mL of D-pantoic acid cyclization reaction liquid, controlling the temperature to be 25-35 ℃, extracting for 10-15 min by using 200mL of ethyl acetate each time, standing for 25-30 min, separating out an organic phase, extracting for 3 times, combining the organic phases extracted for the first 2 times, standing, separating out an aqueous phase, combining the aqueous phases, extracting for the third time, and using the organic phase extracted for the third time;
s2, controlling the temperature to be 20-30 ℃, decoloring the organic phase with 4g of activated carbon for 45-60 min, and filtering to obtain a decolored solution;
s3, controlling the temperature to be 30-35 ℃, washing for 10-15 min by using 0.5 time of deionized water, standing for 25-30 min, separating out an organic phase, and repeatedly washing for 3 times;
s4, controlling the temperature to be 30-40 ℃, enabling the vacuum degree to be more than or equal to 0.09Mpa, concentrating and recovering ethyl acetate, then heating to 60-70 ℃, and concentrating and removing water to obtain a concentrated solution;
s5, adding ethyl acetate with the volume 1 time that of the cyclization reaction solution to dissolve the concentrated solution;
s6, controlling the temperature to be 20-25 ℃, and concentrating in vacuum to be in a syrup state; after the concentration is finished, discharging and centrifuging to obtain D-pantolactone wet powder;
s7, vacuum degree > 0.09Mpa, vacuum drying at 45-50 deg.C to obtain D-pantolactone 104.4g (water content < 0.5%), yield 87%, purity 99.3%, and specific rotation degree 50.7 deg.
Example four
The invention provides a method for purifying D-pantoic acid lactone, which comprises the following steps:
s1, taking 200mL of D-pantoic acid cyclization reaction liquid, controlling the temperature to be 25-35 ℃, extracting for 10-15 min by using 200mL of ethyl acetate each time, standing for 25-30 min, separating out an organic phase, extracting for 3 times, combining the organic phases extracted for the first 2 times, standing, separating out an aqueous phase, combining the aqueous phases, extracting for the third time, and using the organic phase extracted for the third time;
s2, controlling the temperature to be 20-30 ℃, decoloring the organic phase with 4g of activated carbon for 45-60 min, and filtering to obtain a decolored solution;
s3, controlling the temperature to be 30-35 ℃, washing for 10-15 min by using 0.5 time of deionized water, standing for 25-30 min, separating out an organic phase, and repeatedly washing for 3 times;
s4, controlling the temperature to be 30-40 ℃, enabling the vacuum degree to be more than or equal to 0.09Mpa, concentrating and recovering ethyl acetate, then heating to 60-70 ℃, and concentrating and removing water to obtain a concentrated solution;
s5, adding ethyl acetate with 2 times of the volume of the cyclization reaction solution to dissolve the concentrated solution;
s6, controlling the temperature to be 20-25 ℃, and concentrating in vacuum to be in a syrup state; after the concentration is finished, discharging and centrifuging to obtain D-pantolactone wet powder;
s7, vacuum degree > 0.09Mpa, vacuum drying at 45-50 deg.C to obtain D-pantolactone 105.0g (water content < 0.5%), yield 87.5%, purity 99.5%, and specific rotation 51.1 deg.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.
Claims (8)
1. A method for purifying D-pantoic acid lactone is characterized by comprising the following steps:
s1, extracting the cyclization reaction liquid of the D-pantoic acid by using ethyl acetate;
s2, after extraction is finished, decoloring the extraction liquid by using activated carbon to obtain a decolored liquid;
s3, washing the destaining solution by using deionized water;
s4, recovering ethyl acetate from the concentrated decolorized solution, and removing water to obtain a concentrated solution;
s5, dissolving the concentrated solution by using ethyl acetate;
s6, evaporating and crystallizing to obtain D-pantolactone wet powder;
s7, drying the D-pantoic acid lactone wet powder under the vacuum condition to obtain the D-pantoic acid lactone with the purity of more than or equal to 99 percent.
2. The method for purifying D-pantoic acid lactone according to claim 1, wherein the volume ratio of the ethyl acetate and the cyclization reaction liquid in step S1 is 4: 1-2: 1.
3. The method for purifying D-pantoic acid lactone according to claim 1, wherein the amount of activated carbon used in step S2 is 1% -4% by volume of the cyclization reaction solution.
4. The method for purifying D-pantoic acid lactone according to claim 1, wherein the amount of deionized water and the volume of the cyclization reaction solution in step S3 are 0.5:1 to 1.5:1, and the water jacket is washed with water and extracted with the cyclization reaction solution.
5. The method for purifying D-pantolactone according to claim 1, wherein the concentration temperature in step S4 is 20-70 ℃ and the vacuum degree is not less than 0.09 MPa.
6. The method for purifying D-pantoic acid lactone according to claim 1, wherein the water content of ethyl acetate in step S5 is not more than 0.2%, and the volume ratio of ethyl acetate to the cyclization reaction solution is 0.5: 1-2: 1.
7. The method for purifying D-pantolactone according to claim 1, wherein the evaporation and crystallization temperature of step S6 is 20-30 ℃, and the vacuum degree is not less than 0.09 MPa.
8. The method for purifying D-pantolactone according to claim 1, wherein the vacuum drying temperature in step S7 is 45 to 50 ℃.
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| CN110845307A (en) * | 2019-11-28 | 2020-02-28 | 安徽泰格生物科技有限公司 | A kind of recovery method of D-calcium pantothenate mother liquor |
| CN110862362A (en) * | 2019-11-28 | 2020-03-06 | 安徽泰格生物科技有限公司 | Refining method of D-pantoic acid lactone |
| CN112679453A (en) * | 2020-12-16 | 2021-04-20 | 蚌埠丰原医药科技发展有限公司 | Preparation method of D-pantoic acid lactone |
| CN114934061A (en) * | 2022-05-20 | 2022-08-23 | 中国科学院微生物研究所 | Engineering bacteria and their application in whole-cell catalyzed production of D-pantolactone from ketopantolactone |
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