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The preparation method of ethyl isopentyl malonate diethyl ester

A technology of diethyl ethyl isopentyl malonate and diethyl ethyl malonate, which can be used in the preparation of carboxylic acid esters, organic compounds, metal alcohols, etc., and can solve the problem of low yield and purity etc. to achieve the effect of high purity and high yield

Active Publication Date: 2018-02-13
WEIFANG JINGRUN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] In view of this, the purpose of this invention is to provide a kind of preparation method of ethyl isopentyl diethyl malonate, which solves the technical problem that the existing method yield and purity are low

Method used

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  • The preparation method of ethyl isopentyl malonate diethyl ester
  • The preparation method of ethyl isopentyl malonate diethyl ester

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preparation example Construction

[0015] A preparation method of diethyl ethyl isopentyl malonate, comprising the following steps:

[0016] 1) Ethanol and sodium react to generate sodium ethylate

[0017] 2) adding diethyl ethylmalonate to the sodium ethylate obtained in step 1), generating diethyl ethylmalonate sodium salt;

[0018] 3) Add bromoisopentane to the diethyl ethylmalonate sodium salt obtained in step 2), and react to generate diethyl ethylmalonate.

[0019] The invention uses ethanol, sodium, diethyl ethylmalonate and bromoisopentane as raw materials to prepare diethyl ethylisoamylmalonate with high yield and high purity, and meets the quality standard of medicines.

[0020] Wherein, the reaction of ethanol and sodium generates the reaction formula of sodium ethylate as follows:

[0021] Na+C 2 h 5 OH→C 2 h 5 ONa+H 2 ↑.

[0022] In the embodiment of the present invention, the preparation of sodium ethylate is in N 2 Prepared under atmosphere, avoiding the problem of easy decomposition and...

Embodiment 1

[0034] Feed N into the reactor containing 1200g ethanol 2 , add 80g of sodium to absolute ethanol, at 72°C, after 12h of reaction, stop feeding N 2 ; At the same time, heat the temperature to 80°C to remove ethanol to obtain sodium ethylate; then pass cooling water into the cooling water jacket of the reactor for 30 minutes, and then pass into N 2 , and slowly add 600g diethyl ethyl malonate dropwise to sodium ethylate, stop feeding cooling water and N 2 , to obtain diethyl ethyl malonate sodium salt; 450g of bromoisopentane was added dropwise, and kept at 76°C for 30min, filtered and rectified to obtain diethyl ethyl malonate.

[0035] The yield of diethyl ethyl isopentyl malonate prepared in this example was 83.33%, and the purity was 99.52%.

Embodiment 2

[0037] Feed N into the reactor containing 1350g ethanol 2 , add 82g of sodium to absolute ethanol, at 73°C, after reacting for 13h, stop feeding N 2 At the same time, heat the temperature to 80°C to remove ethanol to obtain sodium ethylate; then pass cooling water into the cooling water jacket of the reactor for 60 minutes, and then pass into N 2 , and slowly add 600g diethyl ethyl malonate dropwise to sodium ethylate, stop feeding cooling water and N 2 , to obtain diethyl ethyl malonate sodium salt; 460g of bromoisopentane was added dropwise, and kept at 80°C for 45min, filtered and rectified to obtain diethyl ethyl isopentyl malonate.

[0038] The yield of diethyl ethyl isopentyl malonate prepared in this example was 82.95%, and the purity was 99.54%.

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Abstract

The invention discloses a preparation method of diethyl ethylisopentylmalonate. The preparation method comprises following steps: 1), ethanol and sodium react to generate sodium ethoxide; 2), diethyl ethylmalonate is added to sodium ethoxide obtained in the step 1), and diethyl ethylmalonate sodium salt is generated; 3), 1-bromo-3-methylbutane is added to the diethyl ethylmalonate sodium salt obtained in the step 2), and diethyl ethylisopentylmalonate is generated after reaction. Diethyl ethylisopentylmalonate is prepared from ethanol, sodium, diethyl ethylmalonate and 1-bromo-3-methylbutane as the raw materials, and prepared diethyl ethylisopentylmalonate has high yield and high purity and meets the drug quality standard.

Description

technical field [0001] The invention relates to the field of diethyl ethyl isopentyl malonate, in particular to a preparation method of diethyl ethyl isopentyl malonate. Background technique [0002] Diethyl ethyl isopentyl malonate is an important pharmaceutical intermediate, its structural formula is as follows: It is mainly used as an intermediate of amobarbital. At present, isoamyl alcohol is usually brominated with hydrobromic acid-sulfuric acid to generate 1-bromo-3-methylbutane, and then condensed with diethyl malonate under the participation of sodium ethoxide to obtain α-isoamylpropanedi Acid diethyl ester, and then the latter and ethyl bromide in the presence of sodium ethylate to participate in the preparation of condensation. But the yield and the purity of the diethyl ethyl isopentyl malonate prepared by the above scheme are relatively low, which greatly affects the quality of downstream medicines. Contents of the invention [0003] In view of this, the pu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/30C07C67/343C07C69/38C07C29/70C07C31/30
CPCC07C29/70C07C67/30C07C67/343C07C69/38C07C31/30
Inventor 郭新平
Owner WEIFANG JINGRUN CHEM CO LTD
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