Preparation method for succinic acid monoethyl ester acyl chloride

A technology for monoethyl succinate acid chloride and crude monoethyl ester acid chloride, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc. The problems of low purity and high production cost can save the solvent separation and recovery process, improve the reaction rate and improve the utilization rate.

Inactive Publication Date: 2012-01-18
HUBEI MEIKAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The biggest disadvantage of this process is high production cost and low product yield
[0006] The above two methods have shortcomings such as low product purity, high content of thionyl chloride and chlorine elements, and unstable quality, which cannot meet the requirements of foreign customers.

Method used

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  • Preparation method for succinic acid monoethyl ester acyl chloride
  • Preparation method for succinic acid monoethyl ester acyl chloride
  • Preparation method for succinic acid monoethyl ester acyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Put 50kg of absolute ethanol into the esterification reactor for the first time, then put 160kg of succinic anhydride into it at a stirring speed of 82r / m, continue stirring, heat up to 76°C and keep warm for esterification reaction, and the reaction time is 30 minutes. Pump another 40kg of absolute ethanol to the dripping tank, and drop it all into the above-mentioned esterification reaction kettle at a rate of 20kg / h at a temperature of 75-78°C to continue the esterification reaction. After the addition is completed, Then, under the condition of 75-78° C., reflux and heat preservation were carried out for esterification reaction for 90 minutes to obtain monoethyl succinate with a content of 98.35%.

[0023] Monoethyl succinate is transferred to the acylation reactor, 2,2-dimethyl-3-(2,2-dichlorovinyl)cyclopropanecarboxylic acid chloride 4kg is added thereto, and thionyl chloride 300kg is extracted in In the dropping tank, add thionyl chloride dropwise at a rate of 100...

Embodiment 2～3

[0031] Keep the feed intake of succinic anhydride 160kg, thionyl chloride 300kg, and catalyst 4kg constant, change the feed intake of dehydrated alcohol, add dehydrated ethanol dropwise for the second time and add dehydrated alcohol mass ratio 1: 1.25 for the first time. Change, other operating conditions and product characterization methods are all the same as in Example 1 to obtain monoethyl succinic acid chloride. The dosage and test results of absolute ethanol are shown in Table 2.

[0032] Table 2. The feeding amount and test result of embodiment 2~3 dehydrated alcohol

[0033]

Embodiment 4～5

[0035] Keep 160kg of succinic anhydride, 90kg of absolute ethanol total amount (the second time is 1: 1.25 for the first time mass ratio), the feed intake of catalyst 4kg is constant, change the feed intake of thionyl chloride, other operating conditions and products The characterization methods were all the same as in Example 1 to obtain monoethyl succinic acid chloride. The dosage and test results of thionyl chloride are shown in Table 3.

[0036] Table 3. The feeding amount and test result of embodiment 4~5 thionyl chloride

[0037]

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Abstract

The invention discloses a preparation method for succinic acid monoethyl ester acyl chloride. The method comprises the following steps of: mixing a certain amount of absolute ethanol and succinic anhydride; performing heat-preserving esterification at the temperature of between 75 and 78 DEG C with stirring for 20 to 40 minutes; adding the absolute ethanol dropwise into the reaction system to continue the esterification; performing reflux heat-preserving reaction at the temperature of between 75 and 80 DEG C for 80 to 100 minutes to obtain succinic acid monoethyl ester; adding a certain amount of 2,2-dimethyl-3-(2,2-dichloro vinyl) cyclopropane carboxyl aryl chloride into the succinic acid monoethyl ester; adding sulfoxide chloride dropwise to start acylation reaction; after the step of adding sulfoxide chloride dropwise is finished, heating to 58 to 62 DEG C and preserving heat to continue the acylation reaction for 110 to 130 minutes to obtain succinic acid monoethyl ester acyl chloride crude products; and purifying the crude products to obtain the succinic acid monoethyl ester acyl chloride. The method is simple, safe and convenient in operation, low in cost, light in environmental pollution and high in yield and purity of products.

Description

technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, in particular to a preparation method of monoethyl succinate chloride. Background technique [0002] Ethyl succinate chloride is light yellow or colorless transparent liquid, also known as ethyl succinate chloride, is a pharmaceutical intermediate, mainly used in the production of erythromycin ethyl succinate, succinic acid and other products, and also used in The production of national second-class new drug dirithromycin and thyroxine drugs such as methimazole, methotrexate, and Jiayuanping drugs can also be used in the production of pesticides. [0003] There are two methods for industrialized production of ethyl succinate chloride at present: [0004] The first method is to use absolute ethanol as a reactant and also as a solvent, and after succinic anhydride and absolute ethanol carry out esterification reaction, carry out acylation reaction with thionyl chloride. Sin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/313
Inventor 胡林松王志刚李小林阮长友张兴江王勇超
Owner HUBEI MEIKAI CHEM
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