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Method for synthesizing malonic ester by one-pot carbonylation

A malonate ester and chemical synthesis technology, which is applied in the direction of carbon monoxide or formate reaction preparation, organic chemistry, etc., can solve the problems of long process flow, decomposition under reduced pressure, and high cost, and achieve simple operation, low production cost, The effect of short production process

Inactive Publication Date: 2013-11-27
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The method has a high conversion rate and mild reaction conditions, but the method has a long technical process step by step and consumes a lot of money. It also uses a large amount of thiosulfate. In addition, due to the instability of cobalt carbonyl, it is easy to decompose under reduced pressure. Therefore, it is difficult to popularized in industry

Method used

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  • Method for synthesizing malonic ester by one-pot carbonylation
  • Method for synthesizing malonic ester by one-pot carbonylation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Use Zn powder as the reducing agent, and feed according to the molar ratio of zinc and cobalt chloride as 1: 3. 0.96g (0.0040mol) CoCl 2 ﹒ 6H 2 O, 0.52g (0.0080mol) Zn powder, 1.5g (0.011mol) K 2 CO 3 , 23ml (0.394mol) of ethanol and 2ml (0.019mol) of ethyl chloroacetate were added to a 50ml stainless steel reaction kettle with a polytetrafluoroethylene lining, and the air in the kettle was replaced with CO for three times, and then flushed into CO to maintain the pressure 1.2MPa, heated up to 65°C, stirred magnetically for 3 hours, and cooled naturally to room temperature under the protection of carbon monoxide. The composition of the reactor liquid was analyzed by gas chromatography. The conversion rate of ethyl chloroacetate was 97%, and the conversion rate of dimalonate Ethyl ester selectivity was 100%.

Embodiment 2

[0021] With Zn powder as reducing agent, and according to the mol ratio of zinc and cobalt chloride is 1: 1 feed, CoCl 2 ﹒ 6H 2 O-catalyzed carbonylation of ethyl chloroacetate with carbon monoxide for one-pot synthesis of diethyl malonate.

[0022] Others are the same as embodiment 1. The composition of the reactor liquid was analyzed by gas chromatography, the conversion rate of ethyl chloroacetate was 90%, and the selectivity of diethyl malonate was 100%.

Embodiment 3

[0024] With Zn powder as reducing agent, and according to the mol ratio of zinc and cobalt chloride is 0.25: 1 feeding, after magnetic stirring 8 hours, CoCl 2 ﹒ 6H 2 O-catalyzed carbonylation of ethyl chloroacetate with carbon monoxide for one-pot synthesis of diethyl malonate.

[0025] Others are the same as embodiment 1. The composition of the reactor liquid was analyzed by gas chromatography, and the conversion rate of ethyl chloroacetate was 85%, and the selectivity of diethyl malonate was 100%.

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Abstract

The invention discloses a method for synthesizing malonic ester by one-pot carbonylation, which is characterized in that: under the conditions of a temperature at 40-80 DEG C and a pressure of carbon monoxide at 0.5-4 MPa, cobalt salts, zinc powders or iron powders, acetate chloride, C1-C6 alcohols and alkalis are added into a carbonylation reaction kettle. The one-pot method for synthesizing the malonic ester reaches a total conversation rate of the acetate chloride of 100% and a total selectivity of the malonic ester of 100%. The method disclosed by the method avoids the pre-preparation technological progress of carbonyl cobalt, is high in yield, gentle in reaction condition, simple and easy in technology.

Description

technical field [0001] The invention relates to a method for preparing malonate, in particular to a method for synthesizing malonate by one-pot carbonylation of chloroacetate and carbon monoxide. Background technique [0002] Malonate is an extremely important fine chemical raw material, due to the active methylene (-CH 2 The hydrogen on -) is easily replaced by a variety of groups, and then undergoes various substitution reactions such as alkylation, alkoxylation, acylation, hydroxylation, and amidation, and generates a variety of important derivatives, so it is widely used It is used in chemical production fields such as pharmaceuticals, pesticides, dyes, and food. [0003] The existing preparation methods of malonate mainly include two kinds of "cyanidation esterification method" and "catalytic carbonylation method". , hydrolysis, esterification and other steps, first neutralized by chloroacetic acid and sodium carbonate to generate sodium chloroacetate, then cyanided w...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/38C07C67/36
Inventor 李福祥霍素芳于峰薛建伟吕志平
Owner TAIYUAN UNIV OF TECH
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