CN106008580A - Purification technology of phenylboronic acid - Google Patents
Purification technology of phenylboronic acid Download PDFInfo
- Publication number
- CN106008580A CN106008580A CN201610436990.2A CN201610436990A CN106008580A CN 106008580 A CN106008580 A CN 106008580A CN 201610436990 A CN201610436990 A CN 201610436990A CN 106008580 A CN106008580 A CN 106008580A
- Authority
- CN
- China
- Prior art keywords
- separation
- solution
- conducted
- column chromatography
- phenylboronic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- HXITXNWTGFUOAU-UHFFFAOYSA-N phenylboronic acid Chemical compound OB(O)C1=CC=CC=C1 HXITXNWTGFUOAU-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000000746 purification Methods 0.000 title abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 17
- 238000004440 column chromatography Methods 0.000 claims abstract description 9
- 239000012535 impurity Substances 0.000 claims abstract description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 125000003963 dichloro group Chemical group Cl* 0.000 claims abstract description 8
- MZRVEZGGRBJDDB-UHFFFAOYSA-N n-Butyllithium Substances [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000009835 boiling Methods 0.000 claims abstract description 4
- 239000006227 byproduct Substances 0.000 claims abstract description 4
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 4
- 239000003208 petroleum Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 9
- 150000002367 halogens Chemical class 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000010992 reflux Methods 0.000 abstract 2
- -1 butyl lithium halogen Chemical class 0.000 abstract 1
- 238000005695 dehalogenation reaction Methods 0.000 abstract 1
- 230000000717 retained effect Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic Table
- C07F5/02—Boron compounds
- C07F5/025—Boronic and borinic acid compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a purification technology of phenylboronic acid, and relates to the technical field of purification. The purification technology comprises the steps that 1, impurity washing is conducted, wherein phenylboronic acid with impurities is mixed with butyl lithium halogen, stirring is conducted through stirring equipment, and after stirring is finished, a dehalogenation by-product is washed by dichloro or petroleum ether; 2, column chromatography separation is conducted, wherein column chromatography separation is conducted on the solution obtained in the step 1, and the solution which is not subjected to column chromatography separation is collected during separation; 3, refluxing is conducted, wherein dichloro is dropwise added into the solution obtained in the step 2, the impurities are separated by a reflux device, and pure phenylboronic acid is retained; 4, the solution collected in the step 2 is subjected to boiling and washing separation. According to the purification technology, raw materials and time can be saved, operation is easy and convenient, and the efficiency and the purity are high.
Description
Technical field
The present invention relates to purification technique field, be specifically related to the purifying technique of a kind of phenylboric acid.
Background technology
Purify and refer to out with this, magazins' layout in mixture is improved its purity；Purify as a kind of important chemical method, not only there is in chemical research important function, have a very important role too in Chemical Manufacture；The most important chemical research and Chemical Manufacture, all to purify；When existing phenylboric acid purifies, its consumption of raw materials is big, and purity is low, in-convenience in use, lose time.
Summary of the invention
Present invention aims to defect and the deficiency of prior art, it is provided that the purifying technique of a kind of phenylboric acid.
In order to solve the problem existing for background technology, the purifying technique of a kind of phenylboric acid of the present invention, its purifying technique is:
Step one, wash impurity: the phenylboric acid with impurity is pulled out halogen with butyl lithium and mixes, be stirred through mixing plant, after stirring, use dichloro even petroleum ether that dehalogenated by-product is washed away；
Step 2, column chromatography for separation: solution in step one is carried out column chromatography for separation, collect the solution not having post during separation；
Step 3, backflow: the solution in step 2 is dripped dichloro, by return channel by magazins' layout, remaining as purer phenylboric acid；
Step 4, by step 2 collect solution carry out boiling washing separation.
Present invention have the beneficial effect that raw material and the time can saved, easy and simple to handle, efficiency is high, and purity is high.
Detailed description of the invention
This detailed description of the invention adopts the following technical scheme that its purifying technique is:
Step one, wash impurity: the phenylboric acid with impurity is pulled out halogen with butyl lithium and mixes, be stirred through mixing plant, after stirring, use dichloro even petroleum ether that dehalogenated by-product is washed away；
Step 2, column chromatography for separation: solution in step one is carried out column chromatography for separation, collect the solution not having post during separation；
Step 3, backflow: the solution in step 2 is dripped dichloro, by return channel by magazins' layout, remaining as purer phenylboric acid；
Step 4, by step 2 collect solution carry out boiling washing separation.
The above, only in order to technical scheme to be described and unrestricted, other amendment or equivalent that technical scheme is made by those of ordinary skill in the art, without departing from the spirit and scope of technical solution of the present invention, all should contain in the middle of scope of the presently claimed invention.
Claims (1)
1. the purifying technique of a phenylboric acid, it is characterised in that: its purifying technique is:
Step one, wash impurity: the phenylboric acid with impurity is pulled out halogen with butyl lithium and mixes, be stirred through mixing plant, after stirring, use dichloro even petroleum ether that dehalogenated by-product is washed away；
Step 2, column chromatography for separation: solution in step one is carried out column chromatography for separation, collect the solution not having post during separation；
Step 3, backflow: the solution in step 2 is dripped dichloro, by return channel by magazins' layout, remaining as purer phenylboric acid；
Step 4, by step 2 collect solution carry out boiling washing separation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610436990.2A CN106008580A (en) | 2016-06-20 | 2016-06-20 | Purification technology of phenylboronic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610436990.2A CN106008580A (en) | 2016-06-20 | 2016-06-20 | Purification technology of phenylboronic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106008580A true CN106008580A (en) | 2016-10-12 |
Family
ID=57088552
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610436990.2A Pending CN106008580A (en) | 2016-06-20 | 2016-06-20 | Purification technology of phenylboronic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106008580A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289033A (en) * | 2013-04-08 | 2013-09-11 | 西安交通大学 | Aryl boron-containing phenolic resin and preparation method thereof |
| EP2862864A1 (en) * | 2013-10-18 | 2015-04-22 | Yriel | Continuous method for preparing boronic acids and derivatives thereof |
-
2016
- 2016-06-20 CN CN201610436990.2A patent/CN106008580A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289033A (en) * | 2013-04-08 | 2013-09-11 | 西安交通大学 | Aryl boron-containing phenolic resin and preparation method thereof |
| EP2862864A1 (en) * | 2013-10-18 | 2015-04-22 | Yriel | Continuous method for preparing boronic acids and derivatives thereof |
Non-Patent Citations (1)
| Title |
|---|
| DAGFINN SLEVELAND ET AL.: ""Synthesis of Phenylboronic Acids in Continuous Flow by Means of a Multijet Oscillating Disc Reactor System Operating at Cryogenic Temperatures"", 《ORGANIC PROCESS RESEARCH & DEVELOPMENT》 * |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161012 |