반응 #3285

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

2-(aminomethyl)pyridine

→

pure product

수율 38.7%

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

수율 38.7%

용매

dimethylformamide

반응 조건

후처리

1. 1
   온도was heated
2. 2
   workup.WAITAfter 2 hours
3. 3
   기타the 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
   여과the entire mixture was filtered
7. 7
   세척The cake was washed 5 mL of ether, 5 mL of water
8. 8
   기타dried
9. 9
   기타Recrystallization from ethyl acetate

실험 절차

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.

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