반응 #3278

반응 방정식

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

용매

Dimethylformamide

반응 조건

후처리

1. 1
   온도The tube was cooled in a dry ice-acetone bath
2. 2
   기타condensed in the tube
3. 3
   기타the tube was closed
4. 4
   온도the reaction mixture was heated behind a shield in a 110° C. oil bath
5. 5
   온도The solution was heated in the oil bath for 20 hours
6. 6
   온도The tube was cooled in an ice-acetone bath
7. 7
   온도warmed to room temperature
8. 8
   기타Most of the dimethylformamide was evaporated at reduced pressure
9. 9
   기타to yield crystals
10. 10
    기타The solid was triturated with 5 mL of water
11. 11
    여과filtered
12. 12
    세척washed with water
13. 13
    기타dried
14. 14
    기타Purification
15. 15
    기타was effected by recrystallization from ethyl acetate-petroleum ether

실험 절차

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.

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