Reaktion #1977421

Reaktionsgleichung

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

ammonia

→

product

Ausbeute 44.0%

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

Ausbeute 44.0%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe cooled solution was evaporated
2. 2
   Sonstigeto remove solvent
3. 3
   ExtraktionAfter an acido-basic work-up and extraction with dichloromethane
4. 4
   Waschenthe mixture was washed with saturated solution of sodium chloride
5. 5
   TrocknenThe organic phase was dried over sodium sulfate
6. 6
   Einengenconcentrated

Vorschrift

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.

Quelle