反応 #8812

反応方程式

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

収率 69.3%

溶媒

methanol

反応条件

後処理

1. 1
   温度the mixture was heated
2. 2
   温度to reflux for 12 h
3. 3
   その他The catalyst was removed by filtration
4. 4
   洗浄washed with MeOH
5. 5
   濃縮the filtrate was concentrated
6. 6
   洗浄Flash column chromatography eluting with 5% MeOH/CH2Cl2 containing 0.5% of NH4OH

実験手順

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.

出典