تفاعل #2427

معادلة التفاعل

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

HBr

→

foam

المردود 91.0%

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

المردود 91.0%

المذيبات

DCM

ظروف التفاعل

المعالجة

1. 1
   أخرىThe solvent was evaporated
2. 2
   أخرىthe product partitioned between 1M HCl and EtOAc
3. 3
   استخلاصextracted with CHCl3 (×3)
4. 4
   غسيلwashed with brine
5. 5
   أخرىdried
6. 6
   أخرىevaporated

الإجراء التجريبي

(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.

المصدر