反応 #3278

反応方程式

6-(2,6-dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one

6-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfanyl-8H-pyrido[2,3-d]pyrimidin-7-one

monomethylamine

→

pure product

6-(2,6-Dichlorophenyl)-8-methyl-2-methylamino-8H-pyrido[2,3-d]pyrimidin-7-one

溶媒

Dimethylformamide

反応条件

後処理

1. 1
   温度The tube was cooled in a dry ice-acetone bath
2. 2
   その他condensed in the tube
3. 3
   その他the tube was closed
4. 4
   温度the reaction mixture was heated behind a shield in a 110° C. oil bath
5. 5
   温度The solution was heated in the oil bath for 20 hours
6. 6
   温度The tube was cooled in an ice-acetone bath
7. 7
   温度warmed to room temperature
8. 8
   その他Most of the dimethylformamide was evaporated at reduced pressure
9. 9
   その他to yield crystals
10. 10
    その他The solid was triturated with 5 mL of water
11. 11
    ろ過filtered
12. 12
    洗浄washed with water
13. 13
    その他dried
14. 14
    その他Purification
15. 15
    その他was effected by recrystallization from ethyl acetate-petroleum ether

実験手順

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.

出典