Synthesis method of dasatinib intermediate
A technology of dasatinib and a synthesis method, applied in the field of drug synthesis, can solve the problems of difficult condensation reaction, large environmental pressure, many by-products, etc., and achieve the effects of easy industrial production, avoiding waste of raw materials, and simple raw materials
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Embodiment 1
[0024] (1) Add 500ml of chloroform, 60g of 2-methyl-4-amino-6-chloropyrimidine, 71.2g of bis(2-chloroethyl)amine, and 87g of potassium carbonate to a 1000ml reaction flask, start stirring, and heat to reflux for 5 After being down to room temperature, the insoluble solids were removed by filtration, and the filtrate was washed with 200ml of saturated sodium chloride solution;
[0025] (2) Then add 40.4g of 2-chloroethanol and 63g of triethylamine to the filtrate, heat and reflux for 4 hours, after the reaction is completed, drop to room temperature, wash with 100ml of hydrochloric acid of 1mol / L, then wash once with 100ml of saturated sodium bicarbonate solution , washed once with 100ml of purified water, then concentrated the organic layer under reduced pressure, added 440g of n-hexane and 110g of ethyl acetate, heated to 50°C, stirred for 1 hour; cooled to 5°C and continued to stir for 30 minutes, suction filtered and dried to obtain 91.5g Off-white solid with a yield of 85....
Embodiment 2
[0027] (1) Add 500ml of chloroform, 60g of 2-methyl-4-amino-6-chloropyrimidine, 71.0g of bis(2-chloroethyl)amine, and 85g of potassium carbonate to a 1000ml reaction bottle, start stirring, and heat to reflux for reaction 6 After being down to room temperature, the insoluble solids were removed by filtration, and the filtrate was washed with 200ml of saturated sodium chloride solution;
[0028] (2) Then add 40.0g of 2-chloroethanol and 60g of triethylamine to the filtrate, heat and reflux for 5 hours, after the reaction is completed, drop to room temperature, wash with 100ml of hydrochloric acid of 1mol / L, then wash once with 100ml of saturated sodium bicarbonate solution , washed once with 100ml of purified water, then concentrated the organic layer under reduced pressure, added 440g of n-hexane and 110g of ethyl acetate, heated to 50°C, stirred for 1 hour; cooled to 5°C and continued to stir for 30 minutes, suction filtered and dried to obtain 91.2g Off-white solid, yield 85...
Embodiment 3
[0030] (1) Add 500ml of chloroform, 60g of 2-methyl-4-amino-6-chloropyrimidine, 71.8g of bis(2-chloroethyl)amine, and 90g of potassium carbonate to a 1000ml reaction bottle, start stirring, and heat to reflux for 4.5 After being down to room temperature, the insoluble solids were removed by filtration, and the filtrate was washed with 200ml of saturated sodium chloride solution;
[0031] (2) Then add 41.0 g of 2-chloroethanol and 65 g of triethylamine to the filtrate, heat and reflux for 3.5 hours, after the reaction is completed, drop to room temperature, wash with 100 ml of hydrochloric acid of 1 mol / L, then wash once with 100 ml of saturated sodium bicarbonate solution , washed once with 100ml of purified water, then concentrated the organic layer under reduced pressure, added 440g of n-hexane and 110g of ethyl acetate, heated to 50°C, stirred for 1 hour; cooled to 5°C and continued to stir for 30 minutes, suction filtered and dried to obtain 91.8g Off-white solid, yield 85...
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