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Preparation method of trimethyl orthoacetate

A technology of trimethyl orthoacetate and acetonitrile, which is applied in the field of preparation of trimethyl orthoacetate, can solve the problems of easy pollution of the environment, high consumption, low content of trimethyl orthoacetate, etc., and achieves safe preparation method, good economic benefits, The effect of high product purity

Pending Publication Date: 2022-06-10
NANTONG TENDENCI CHEM
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Problems solved by technology

[0005] Yet trimethyl orthoacetate synthesis method can't effectively control the generation of side reaction, causes the content of trimethyl orthoacetate in final product to be very low; Too much, it is easy to pollute the environment, and it is not conducive to saving production costs

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  • Preparation method of trimethyl orthoacetate

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Embodiment Construction

[0021] The technical solutions of the present invention are further described below in conjunction with the embodiments. The technical solutions and related parameters given in the following embodiments are only exemplary, and are intended to be used to explain the present invention, but should not be construed as a limitation of the present invention.

[0022] The present embodiment discloses a preparation method of trimethyl orthoacetate, and the specific operations are as follows:

[0023] Add 41g of acetonitrile, 35g of methanol and 200g of aluminum foil oil to a 500ml round-bottomed flask, slowly introduce 47g of hydrogen chloride, and control the temperature not to exceed 5°C; after the ventilation is completed, slowly heat up to 20°C for 10 hours; After ℃, add ammonia methanol, continue to heat up to 30 ℃, and keep for 8 hours; reduce the temperature and filter to remove ammonia chloride, collect methanol by atmospheric distillation of the filtrate, and continue to dist...

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Abstract

The invention provides a preparation method of trimethyl orthoacetate, which comprises the following steps: introducing hydrogen chloride gas into acetonitrile and methanol in the presence of a solvent, and reacting with aminomethanol to generate a trimethyl orthoacetate product, and continuously evaporating to remove the solvent to obtain pure trimethyl orthoacetate. The yield and yield of trimethyl orthoacetate can be effectively improved, and the preparation method is safe, environmentally friendly, suitable for industrial production and wide in application prospect.

Description

technical field [0001] The invention relates to a preparation method of trimethyl orthoacetate, and belongs to the technical field of organic synthesis. Background technique [0002] Trimethyl orthoacetate, also known as 1,1,1-trimethoxyethane, has the molecular formula C 5 H 12 O 3 It is mainly used as an organic intermediate for the synthesis of medicines and pesticides. It is an important intermediate for the synthesis of pyrethroids such as cypermethrin and kungfu pyrethroid by the Sagami method. It is also the main raw material for the production of medicine, food additives, coatings, spices, etc. [0003] Trimethyl orthoacetate can be obtained by directly reacting methanol and acetonitrile with hydrogen chloride in the presence of a solvent and then reacting with ammonia methanol. The reaction principle is: [0004] [0005] However, the trimethyl orthoacetate synthesis method cannot effectively control the generation of side reactions, which causes the content o...

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Application Information

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IPC IPC(8): C07C41/60C07C43/32C07C257/06
CPCC07C41/60C07C257/06C07C43/32
Inventor 张赟
Owner NANTONG TENDENCI CHEM
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