反应详情

A quantity of 0.165 g (0.47 mmol) of 6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 37 was placed in a pressure tube with a magnetic stirring bar. The tube was cooled in a dry ice-acetone bath and ca. 3 mL of monomethylamine gas was condensed in the tube. Dimethylformamide (1.0 mL) was added, and the tube was closed and allowed to warm to room temperature. With stirring, the reaction mixture was heated behind a shield in a 110° C. oil bath. After 10 minutes, all solid was in solution. The solution was heated in the oil bath for 20 hours. The tube was cooled in an ice-acetone bath, opened, and warmed to room temperature to vent the excess amine. Most of the dimethylformamide was evaporated at reduced pressure to yield crystals. The solid was triturated with 5 mL of water, filtered, washed with water and dried; wt 0.128 g. Purification was effected by recrystallization from ethyl acetate-petroleum ether to give 0.081 g of pure product; mp 243°-244° C.

1. temperatureThe tube was cooled in a dry ice-acetone bath
2. customcondensed in the tube
3. customthe tube was closed
4. temperaturethe reaction mixture was heated behind a shield in a 110° C. oil bath
5. temperatureThe solution was heated in the oil bath for 20 hours
6. temperatureThe tube was cooled in an ice-acetone bath
7. temperaturewarmed to room temperature
8. customMost of the dimethylformamide was evaporated at reduced pressure
9. customto yield crystals
10. customThe solid was triturated with 5 mL of water
11. filtrationfiltered
12. washwashed with water
13. customdried
14. customPurification
15. customwas effected by recrystallization from ethyl acetate-petroleum ether