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Preparation method of diethyl ethoxy methylene malonate

A technology of diethyl ethoxymethylene malonate and diethyl malonate is applied in the field of preparation of diethyl ethoxymethylene malonate, and can solve the problems of high raw material cost and reaction process. complex, harsh reaction conditions, etc., to achieve the effect of easy operation and realization, good atom economy, and simple reaction process

Active Publication Date: 2021-06-04
杭州新本立医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] In summary, there are many deficiencies in the existing process: (1) harsh reaction conditions, high energy consumption and time; (2) poor atom economy, high raw material cost; (3) complex reaction process, not easy to industrial scale-up

Method used

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  • Preparation method of diethyl ethoxy methylene malonate
  • Preparation method of diethyl ethoxy methylene malonate
  • Preparation method of diethyl ethoxy methylene malonate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 68g of sodium ethoxide, 160g of diethyl malonate, 300g of ethanol, and 0.25g of piperidine into the autoclave, start stirring, feed carbon monoxide into the autoclave, ventilate three times, heat, and control the temperature at 100°C. Reach 2MPa, react for 2 hours. After the reaction, the temperature was lowered to room temperature, and the pressure was slowly released to normal pressure to obtain suspension I. Drop the suspension I into 300g of 30% ethanol hydrogen chloride for acidification, and stir at room temperature for 4 hours. Neutralize, filter, and distill under reduced pressure to obtain compound II with a yield of 87.1% and a purity of 98%.

Embodiment 2

[0038] Add 68g of sodium ethoxide, 160g of diethyl malonate, 300g of ethanol, and 0.5g of tetrabutylammonium bromide into the autoclave, start stirring, feed carbon monoxide into the autoclave, ventilate three times, and heat to control the temperature At 100°C, the pressure reached 2MPa, and the reaction was carried out for 2 hours. After the reaction, the temperature was lowered to room temperature, and the pressure was slowly released to normal pressure to obtain suspension I. The suspension I was dropped into 300 g of 30% ethanol hydrogen chloride for acidification, and stirred at room temperature for 4 hours. Neutralization, filtration, and distillation under reduced pressure gave Compound II with a yield of 84.7% and a purity of 97%.

Embodiment 3

[0040] Add 68g of sodium ethoxide, 160g of diethyl malonate, 300g of ethanol, and 0.25g of dibenzo-24-crown-8 into the autoclave, start stirring, pass carbon monoxide into the autoclave, ventilate three times, and heat , the temperature was controlled at 100° C., the pressure reached 2 MPa, and the reaction was carried out for 2 hours. After the reaction, the temperature was lowered to room temperature, and the pressure was slowly released to normal pressure to obtain suspension I. The suspension I was dropped into 300 g of 30% ethanol hydrogen chloride for acidification, and stirred at room temperature for 4 hours. Neutralization, filtration, and vacuum distillation gave Compound II with a yield of 91.8% and a purity of 99%. The GC chart of the reaction solution is attached figure 1 As shown, the corresponding data are shown in Table 1, where the retention time is 5.901 for diethyl malonate, and the retention time is 12.617 for the product. The gc diagram of the purified pr...

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Abstract

The invention discloses a preparation method of ethyoxyl methylene diethyl malonate, and the method comprises the following steps: taking diethyl malonate as a raw material and ethyl formate or carbon monoxide as an auxiliary material, introducing formyl under the action of a catalyst, and carrying out condensation reaction with alcohol under the catalysis of acid to obtain the product ethyoxyl methylene diethyl malonate, wherein ethyl formate can be replaced by CO, and the raw material cost is lower. The method has the advantages of simple operation, easily available raw materials, high conversion rate, safety, environmental protection and low cost, and can realize industrial production.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a preparation method of diethyl ethoxymethylene malonate. Background technique [0002] Diethyl ethoxymethylenemalonate, also known as EMME, contains multiple active groups and is an important intermediate in pharmaceutical and chemical industries. It is widely used and is an important intermediate for the preparation of heterocyclic compounds. [0003] Exist the synthetic method of multiple ethoxymethylene malonate diethyl ester at present, more typical is following two kinds of methods: [0004] The first method is Organic Syntheses, Coll.Vol.3, p.395 (1955); Vol.28, p.60 (1948) literature report, disclosed in this open document with diethyl malonate and Triethyl orthoformate as raw material, in ZnCl 2 , Synthesis of diethyl ethoxymethylene malonate under the catalysis of acetic anhydride. [0005] Its chemical reaction formula is as follows: [0006] [0007]...

Claims

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Application Information

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IPC IPC(8): C07C67/31C07C69/734
CPCC07C67/31C07C69/734
Inventor 顾海宁蒋誉
Owner 杭州新本立医药有限公司
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