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Preparation method of diethyl n-butylmalonate

A technology of diethyl n-butylmalonate and diethyl malonate, which is applied in the field of preparation of diethyl n-butylmalonate, can solve the problem of increasing the production cost of diethyl n-butylmalonate and other problems, to achieve the effect of reducing production cost, high yield and high purity

Inactive Publication Date: 2016-06-08
WEIFANG JINGRUN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of diethyl n-butylmalonate usually requires the use of a catalyst to obtain diethyl n-butylmalonate of high yield, and the use of a catalyst will inevitably increase the preparation cost of diethyl n-butylmalonate

Method used

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  • Preparation method of diethyl n-butylmalonate
  • Preparation method of diethyl n-butylmalonate

Examples

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preparation example Construction

[0016] A preparation method for n-butyl malonate, comprising the following steps:

[0017] 1) ethanol and sodium react to generate sodium ethylate;

[0018] 2) adding diethyl malonate to the sodium ethylate obtained in step 1), generating diethyl malonate sodium salt;

[0019] 3) Add bromobutane to the diethyl malonate sodium salt obtained in step 2), and react to generate n-butyl diethyl malonate.

[0020] The present invention uses ethanol, sodium, diethyl malonate and bromobutane as raw materials without catalyst, reduces the cost of n-butyl diethyl malonate, and the yield of n-butyl diethyl malonate High, high purity, in line with drug quality standards.

[0021] Wherein, the reaction of ethanol and sodium generates the reaction formula of sodium ethylate as follows:

[0022] Na+C 2 h 5 OH→C 2 h 5 ONa+H 2 ↑.

[0023] In the embodiment of the present invention, the preparation of sodium ethylate is in N 2 Prepared under atmosphere, avoiding the problem of easy dec...

Embodiment 1

[0035] Feed N into the reaction kettle filled with 900g ethanol 2 , add 90g of sodium to absolute ethanol, and after reacting for 12h at 73°C, 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 malonate dropwise to sodium ethylate, stop feeding cooling water and N 2 , to obtain diethyl malonate sodium salt; 590g of bromobutane was added dropwise, and kept at 76°C for 30 minutes, filtered and rectified to obtain diethyl n-butylmalonate.

[0036] The yield of diethyl n-butylmalonate prepared in this example was 76.42%, and the purity was 99.57%.

Embodiment 2

[0038] Feed N into the reactor containing 1200g ethanol 2 , add 96g of sodium to absolute ethanol, at 73°C, after 14h 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 60 minutes, and then pass into N 2 , and slowly add 600g diethyl malonate dropwise to sodium ethylate, stop feeding cooling water and N 2 , to obtain diethyl malonate sodium salt; 600g of bromobutane was added dropwise, and kept at 80°C for 45min, filtered and rectified to obtain diethyl n-butyl malonate.

[0039] The yield of diethyl n-butylmalonate prepared in this example was 76.48%, and the purity was 99.69%.

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Abstract

The invention discloses a preparation method of diethyl n-butylmalonate. The preparation method comprises following steps as follows: 1), ethanol and sodium react to generate sodium ethoxide; 2), diethyl malonate is added to sodium ethoxide obtained in the step 1), and diethyl malonate sodium salt is generated; 3), bromobutane is added to the diethyl malonate sodium salt obtained in the step 2), and diethyl n-butylmalonate is generated through reaction. According to the preparation method of diethyl n-butylmalonate, ethanol, sodium, diethyl malonate and bromobutane are taken as raw materials, a catalyst is not required, prepared diethyl n-butylmalonate has high yield and high purity and meets the drug quality standard, and meanwhile, the preparation cost is reduced.

Description

technical field [0001] The invention relates to the field of n-butyl diethyl malonate, in particular to a preparation method of n-butyl diethyl malonate. Background technique [0002] Diethyl n-butylmalonate is an important organic chemical raw material, which is widely used in the fields of dyes, spices, pesticides and medicines, especially in the synthesis of medicines. It is an important synthetic intermediate. Its structural formula as follows: It is mainly used as an intermediate of antipyretic and analgesic phenylbutazone. At present, the preparation of diethyl n-butylmalonate usually requires the use of a catalyst to obtain diethyl n-butylmalonate of high yield, and the use of a catalyst will inevitably increase the preparation cost of diethyl n-butylmalonate . Contents of the invention [0003] In view of this, the purpose of this invention is to provide a kind of preparation method of n-butyl diethyl malonate, which reduces the cost of n-butyl diethyl malonate...

Claims

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Application Information

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IPC IPC(8): C07C67/343C07C69/46
CPCC07C67/343C07C69/46
Inventor 郭新平
Owner WEIFANG JINGRUN CHEM CO LTD
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