반응 #2427

반응 방정식

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

HBr

→

foam

수율 91.0%

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

수율 91.0%

용매

DCM

반응 조건

후처리

1. 1
   기타The solvent was evaporated
2. 2
   기타the product partitioned between 1M HCl and EtOAc
3. 3
   추출extracted with CHCl3 (×3)
4. 4
   세척washed with brine
5. 5
   기타dried
6. 6
   기타evaporated

실험 절차

(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.

출처