반응 #8812

반응 방정식

7-Benzyl-4-morpholin-4-yl-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine

7-benzyl-4-morpholin-4-yl-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine

ammonium formate

→

4-morpholin-4-yl-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine

수율 69.3%

용매

methanol

반응 조건

후처리

1. 1
   온도the mixture was heated
2. 2
   온도to reflux for 12 h
3. 3
   기타The catalyst was removed by filtration
4. 4
   세척washed with MeOH
5. 5
   농축the filtrate was concentrated
6. 6
   세척Flash column chromatography eluting with 5% MeOH/CH2Cl2 containing 0.5% of NH4OH

실험 절차

7-Benzyl-4-morpholin-4-yl-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine 5a (0.55 g, 1.77 mmol) was dissolved in methanol (35 mL) under nitrogen. 10% Pd/C (0.55 g) was added under nitrogen followed by ammonium formate (1.12 g, 17.72 mmol) and the mixture was heated to reflux for 12 h. The catalyst was removed by filtration, washed with MeOH and the filtrate was concentrated. Flash column chromatography eluting with 5% MeOH/CH2Cl2 containing 0.5% of NH4OH gave 0.27 g of 4-morpholin-4-yl-5,6,7,8-tetrahydro-pyrido[3,4-d]pyrimidine 6a as a pale yellow dense liquid.

출처