تفاعل #3278

معادلة التفاعل

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

المذيبات

Dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe tube was cooled in a dry ice-acetone bath
2. 2
   أخرىcondensed in the tube
3. 3
   أخرىthe tube was closed
4. 4
   درجة الحرارةthe reaction mixture was heated behind a shield in a 110° C. oil bath
5. 5
   درجة الحرارةThe solution was heated in the oil bath for 20 hours
6. 6
   درجة الحرارةThe tube was cooled in an ice-acetone bath
7. 7
   درجة الحرارةwarmed to room temperature
8. 8
   أخرىMost of the dimethylformamide was evaporated at reduced pressure
9. 9
   أخرىto yield crystals
10. 10
    أخرىThe solid was triturated with 5 mL of water
11. 11
    ترشيحfiltered
12. 12
    غسيلwashed with water
13. 13
    أخرىdried
14. 14
    أخرىPurification
15. 15
    أخرىwas effected by recrystallization from ethyl acetate-petroleum ether

الإجراء التجريبي

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.

المصدر