反応 #1977421

反応方程式

(+/−)-9-bromo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-7-oxa-1,4a-diaza-benzocyclohepten-4-one

ammonia

→

product

収率 44.0%

(+/−)-9-Amino-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-7-oxa-1,4a-diaza-benzocyclohepten-4-one

収率 44.0%

反応条件

後処理

1. 1
   その他The cooled solution was evaporated
2. 2
   その他to remove solvent
3. 3
   抽出After an acido-basic work-up and extraction with dichloromethane
4. 4
   洗浄the mixture was washed with saturated solution of sodium chloride
5. 5
   乾燥The organic phase was dried over sodium sulfate
6. 6
   濃縮concentrated

実験手順

A suspension of 18.7 g (57.89 mmol) of (+/−)-9-bromo-2-pyrimidin-4-yl-5,6,8,9-tetrahydro-7-oxa-1,4a-diaza-benzocyclohepten-4-one in 520 mL of ammonia (7N solution in MeOH) in sealed tubes was stirred at 100° C. for 4 hours. The cooled solution was evaporated to remove solvent. After an acido-basic work-up and extraction with dichloromethane, the mixture was washed with saturated solution of sodium chloride. The organic phase was dried over sodium sulfate and concentrated. The residue was organised in diethyl ether to afford 6.70 g (44%) of product as a yellow solid.

出典