反応 #2427

反応方程式

(3RS)-Ethyloxycarbonylamino-1-(tert-butylcarbonylmethyl)-2,3-dihydro-5-(2-pyridyl)-1H-1,4-benzodiazepin-2-one

HBr

→

foam

収率 91.0%

(3RS)-Amino-1-(tert-butylcarbonylmethyl)-2,3-dihydro-5-(2-pyridyl)-1H-1,4-benzodiazepin-2-one

収率 91.0%

溶媒

DCM

反応条件

後処理

1. 1
   その他The solvent was evaporated
2. 2
   その他the product partitioned between 1M HCl and EtOAc
3. 3
   抽出extracted with CHCl3 (×3)
4. 4
   洗浄washed with brine
5. 5
   その他dried
6. 6
   その他evaporated

実験手順

(3RS)-Ethyloxycarbonylamino-1-(tert-butylcarbonylmethyl)-2,3-dihydro-5-(2-pyridyl)-1H-1,4-benzodiazepin-2-one (IV, 250 mg, 0.592 mmol) was taken up in dry DCM (10 ml) at 0° C. and saturated with dry HBr gas. The mixture was stoppered and stirred at r.t. for 64 h. The solvent was evaporated and the product partitioned between 1M HCl and EtOAc. The acid portion was basified and extracted with CHCl3 (×3). The extracts were combined and washed with brine, dried and evaporated to give a brown foam (188 mg, 91%), which was not purified further.

出典