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
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[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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