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Synthesis method of 5-iodine-6-methyl nicotinonitrile

A synthetic method, the technology of methylnicotinonitrile, applied in the direction of organic chemistry, etc., can solve the problems of no reported synthetic method, and achieve the effect of simple operation, high yield and easy operation

Pending Publication Date: 2022-07-15
江苏壹药新材料有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] 5-iodo-6-methylnicotinonitrile is an important chemical intermediate, but its synthesis method has not been reported so far

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0018] A synthetic method of 5-iodo-6-methylnicotinonitrile, the synthetic method comprises the steps:

[0019] (1) According to compound A, the solid-liquid g / mL ratio of 25% ammonia water is 1:13, and the volume ratio of ammonia water and ethanol is 2:1, take the material, put compound A, ammonia water and ethanol into the reaction In the device, heat to 120~125℃, set the pressure to 1MPa, and react to obtain compound B;

[0020] (2) According to the mass ratio of compound B and N-iodosuccinimide as 7:13, and the solid-liquid g / mL ratio of compound B and N,N-dimethylformamide as 7:110 , add compound B, N,N-dimethylformamide and N-iodosuccinimide to the reactor, and react to obtain compound C;

[0021] (3) According to the mass ratio of compound C, isoamyl nitrite and copper powder of 6:3 to 5:2, and the solid-to-liquid g / mL ratio of compound C and DMF to 3:50, take the material and put it into the reactor. Add compound C, DMF, isoamyl nitrite, nitrogen protection, heat to ...

Embodiment 1

[0023] A synthetic method of 5-iodo-6-methylnicotinonitrile, the synthetic method comprises the steps:

[0024] (1) Put 15g of compound A, 195mL of ammonia water with a mass fraction of 25%, and 97.5mL of ethanol into the reactor, heat it to 120°C, set the pressure to 1MPa, react for 3h, check by TLC, the raw materials have basically reacted, take out the kettle The reaction solution was concentrated in ethanol, filtered and washed with water to obtain 11.9 g of a yellow solid, that is, compound B was obtained with a yield of 90.9% and a purity of 96.8%;

[0025] (2) Add 7g of compound B, 110mL of N,N-dimethylformamide and 13g of N-iodosuccinimide to the reactor, react for 15h, check by TLC, the reaction of the raw materials is completed, add 300mL of water to the reaction solution , 200 mL of ethyl acetate was stirred for 10 min, celite was added for filtration, the liquid was separated, the aqueous phase was continuously extracted once with 200 mL of ethyl acetate, the organ...

Embodiment 2

[0029] A synthetic method of 5-iodo-6-methylnicotinonitrile, the synthetic method comprises the steps:

[0030] (1) Put 15g of compound A, 195mL of ammonia water with a mass fraction of 25%, and 97.5mL of ethanol into the reactor, heat it to 123°C, set the pressure to 1MPa, react for 3h, check by TLC, the raw materials have basically reacted, take out the kettle The reaction solution was concentrated in ethanol, filtered and washed with water to obtain 12.4 g of a yellow solid, that is, compound B was obtained with a yield of 94.7% and a purity of 97.3%;

[0031] (2) Add 7g of compound B, 110mL of N,N-dimethylformamide and 13g of N-iodosuccinimide to the reactor, react for 15h, check by TLC, the reaction of the raw materials is completed, add 300mL of water to the reaction solution , 200 mL of ethyl acetate was stirred for 10 min, celite was added for filtration, the liquid was separated, the aqueous phase was continuously extracted once with 200 mL of ethyl acetate, the organ...

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PUM

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Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a synthesis method of 5-iodine-6-methyl nicotinonitrile. According to the present invention, the compound A is adopted as the basic raw material, the nucleophilic substitution, the electrophilic substitution and the Sandmeyer reaction are sequentially performed to prepare the 5-iodine-6-methyl nicotinonitrile, and the prepared 5-iodine-6-methyl nicotinonitrile has characteristics of high yield, good purity, simpleness and easy operation.

Description

technical field [0001] The invention belongs to the technical field of compound synthesis, and in particular relates to a method for synthesizing 5-iodo-6-methylnicotinonitrile. Background technique [0002] Niacin is a white crystal. Sublimation, soluble in alcohol, ether, chloroform, benzene and petroleum ether, slightly soluble in water. The main use is as an intermediate for medicine, food additives, feed additives, pesticides, etc. 5-Iodo-6-methylnicotinonitrile is an important derivative of nicotinonitrile. [0003] 5-iodo-6-methylnicotinonitrile is an important chemical intermediate, but no synthetic method has been reported so far. SUMMARY OF THE INVENTION [0004] In view of the above-mentioned problems, the present invention provides a method for synthesizing 5-iodo-6-methylnicotinonitrile with simple operation and high yield. [0005] In order to solve the above-mentioned problems, the technical scheme provided by the present invention is: [0006] A synthe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/85
CPCC07D213/85
Inventor 李小明刘芝英
Owner 江苏壹药新材料有限公司
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