Реакция #1977421

Уравнение реакции

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

ammonia

→

product

Выход 44.0%

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

Выход 44.0%

Условия реакции

Обработка

1. 1
   ДругоеThe cooled solution was evaporated
2. 2
   Другоеto remove solvent
3. 3
   ЭкстракцияAfter an acido-basic work-up and extraction with dichloromethane
4. 4
   Промывкаthe mixture was washed with saturated solution of sodium chloride
5. 5
   СушкаThe organic phase was dried over sodium sulfate
6. 6
   Концентрированиеconcentrated

Методика

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.

Источник