CN1268506A - Preparation method of ethoxymethylidene diethyl malonate - Google Patents
Preparation method of ethoxymethylidene diethyl malonate Download PDFInfo
- Publication number
- CN1268506A CN1268506A CN 00102535 CN00102535A CN1268506A CN 1268506 A CN1268506 A CN 1268506A CN 00102535 CN00102535 CN 00102535 CN 00102535 A CN00102535 A CN 00102535A CN 1268506 A CN1268506 A CN 1268506A
- Authority
- CN
- China
- Prior art keywords
- diethyl malonate
- preparation
- ethoxymethylidene
- triethyl orthoformate
- malonate
- 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
- -1 ethoxymethylidene diethyl Chemical group 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 13
- LTMRRSWNXVJMBA-UHFFFAOYSA-L 2,2-diethylpropanedioate Chemical compound CCC(CC)(C([O-])=O)C([O-])=O LTMRRSWNXVJMBA-UHFFFAOYSA-L 0.000 claims abstract description 10
- GKASDNZWUGIAMG-UHFFFAOYSA-N triethyl orthoformate Chemical compound CCOC(OCC)OCC GKASDNZWUGIAMG-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 238000007086 side reaction Methods 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 2
- GFIIHTNOFVQNFN-UHFFFAOYSA-N 8-ethoxy-1,5-dioxecane-2,4-dione Chemical compound C1(CC(=O)OCCC(CCO1)OCC)=O GFIIHTNOFVQNFN-UHFFFAOYSA-N 0.000 abstract 1
- 238000006482 condensation reaction Methods 0.000 abstract 1
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic acid anhydride Natural products CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 4
- 230000035484 reaction time Effects 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229940078494 nickel acetate Drugs 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The prepn. method of ethoxy methylene diethyl malonate uses mono-component nickel catalyst through the condensation reaction of triethyl ortho formate and diethyl malonate, and then through rectification to obtain high-quality and high-yield ethoxymethylenediethyl malonate. Advantages include little side reaction, good quality, high yield, and no corrosion to equipment, etc..
Description
The invention belongs to the preparation method of ethoxymethylidene diethyl malonate.
Before the present invention makes, at present the suitability for industrialized production of ethoxymethylidene diethyl malonate is to be catalyzer with the two components of nickel acetate, acetic acid or aceticanhydride, excessive greatly triethyl orthoformate and diethyl malonate reaction, long reaction time, side reaction is many, product is difficult to purify, and equipment is had certain corrosion.
Task of the present invention is to be raw material with triethyl orthoformate, diethyl malonate, and the preparation method of the ethoxymethylidene diethyl malonate that a kind of reaction times is short, side reaction is few, product purity is high, yield is high is provided.
The preparation method of ethoxymethylidene diethyl malonate of the present invention, with triethyl orthoformate, diethyl malonate is raw material, adopt nickel catalyzator, in reactor, add triethyl orthoformate, diethyl malonate and nickel catalyzator, 150 ℃～180 ℃ of control temperature in the kettle, tower top temperature is below 80 ℃, and stirring velocity is fully reaction under 11～120 rev/mins of conditions, and the rectification process mixture promptly gets ethoxymethylidene diethyl malonate.The mol ratio of control diethyl malonate and triethyl orthoformate is 1: 1.5～1: 1.
The preparation method of ethoxymethylidene diethyl malonate of the present invention compared with prior art, it is short to have the reaction times, side reaction is few, and equipment is not had corrosion, the product purity height, the yield height, advantage such as easy to implement, economic results in society are remarkable.
Embodiment:
99% triethyl orthoformate 140kg, 99% diethyl malonate 100kg, nickel catalyzator 200g are dropped into reactor in the lump, in normal pressure, tower temperature＜80 ℃, 150 ℃～180 ℃ of still temperature, stirring velocity is reaction 7 hours under 11 rev/mins of conditions, the rectification under vacuum reaction mixture gets 99.5% ethoxymethylidene diethyl malonate 123.8kg, yield 91.7%.
Claims (3)
1, a kind of preparation method of ethoxymethylidene diethyl malonate, with triethyl orthoformate and diethyl malonate is raw material, it is characterized in that adopting the single-component nickel catalyzator, in reactor, add triethyl orthoformate and diethyl malonate and nickel catalyzator, 150 ℃～180 ℃ of control temperature of reaction kettle, tower top temperature reacts fully below 80 ℃, and the rectification under vacuum mixed reaction product promptly gets ethoxymethylidene diethyl malonate.
2, preparation method as claimed in claim 1 is characterized in that adopting the single-component nickel catalyzator.
3, preparation method as claimed in claim 1 is characterized in that controlling diethyl malonate and triethyl orthoformate mol ratio 1: 1.5～1: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00102535 CN1268506A (en) | 2000-03-04 | 2000-03-04 | Preparation method of ethoxymethylidene diethyl malonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00102535 CN1268506A (en) | 2000-03-04 | 2000-03-04 | Preparation method of ethoxymethylidene diethyl malonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1268506A true CN1268506A (en) | 2000-10-04 |
Family
ID=4576450
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00102535 Pending CN1268506A (en) | 2000-03-04 | 2000-03-04 | Preparation method of ethoxymethylidene diethyl malonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1268506A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104284879A (en) * | 2012-05-16 | 2015-01-14 | 索尔维公司 | Manufacture of 1-substituted methylidene compounds |
| CN104860818A (en) * | 2015-04-20 | 2015-08-26 | 浙江新和成股份有限公司 | Synthesizing method of diethyl ethoxy-methylene malonate |
| CN111440160A (en) * | 2020-04-26 | 2020-07-24 | 黑龙江省绥化农垦晨环生物制剂有限责任公司 | A kind of preparation method of oxaflutole and application thereof |
| CN112062692A (en) * | 2019-06-11 | 2020-12-11 | 太仓市茜泾化工有限公司 | Preparation method of ethyl ethoxymethylene cyanoacetate |
-
2000
- 2000-03-04 CN CN 00102535 patent/CN1268506A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104284879A (en) * | 2012-05-16 | 2015-01-14 | 索尔维公司 | Manufacture of 1-substituted methylidene compounds |
| CN104860818A (en) * | 2015-04-20 | 2015-08-26 | 浙江新和成股份有限公司 | Synthesizing method of diethyl ethoxy-methylene malonate |
| CN112062692A (en) * | 2019-06-11 | 2020-12-11 | 太仓市茜泾化工有限公司 | Preparation method of ethyl ethoxymethylene cyanoacetate |
| CN111440160A (en) * | 2020-04-26 | 2020-07-24 | 黑龙江省绥化农垦晨环生物制剂有限责任公司 | A kind of preparation method of oxaflutole and application thereof |
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