تفاعل #3285

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

2-(aminomethyl)pyridine

→

pure product

المردود 38.7%

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

المردود 38.7%

المذيبات

dimethylformamide

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   workup.WAITAfter 2 hours
3. 3
   أخرىthe excess amine and dimethylformamide were evaporated at reduced pressure
4. 4
   workup.ADDITIONEther (5 mL) was added to the residue
5. 5
   workup.ADDITIONWater (5 mL) was added
6. 6
   ترشيحthe entire mixture was filtered
7. 7
   غسيلThe cake was washed 5 mL of ether, 5 mL of water
8. 8
   أخرىdried
9. 9
   أخرىRecrystallization from ethyl acetate

الإجراء التجريبي

A mixture 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, 1.08 g (10.0 mmol) of 2-(aminomethyl)pyridine and 0.5 mL of dimethylformamide was heated with stirring in a 130° C. oil bath. After 2 minutes, solution was complete. After 2 hours, the excess amine and dimethylformamide were evaporated at reduced pressure. Ether (5 mL) was added to the residue. Crystals immediately developed. Water (5 mL) was added, and the entire mixture was filtered. The cake was washed 5 mL of ether, 5 mL of water, and then dried; wt 0.164 g. Recrystallization from ethyl acetate gave 0.075 g of pure product; mp 198°-201° C.

المصدر