HRID743699

反应详情

EQUATION

反应方程式

HRID 743699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3(R,S)-[(Benzyloxycarbonyl)amino]-5-cycloheptyl-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one (435 mg) was treated with a solution of 30% hydrogen bromide in glacial acetic add (10 ml) and stirred for 20 min at room temperature. The mixture was then added dropwise onto cold (0° C.) diethyl ether (50 ml). A white solid precipitated which was filtered off. The solid was treated with 10% sodium hydroxide solution (50 ml), then extracted with ethyl acetate (80 ml). The organic layer was separated, dried (Na2SO4) and evaporated to give crude 3(R,S)-amino-5-cycloheptyl-1,3-dihydro-1-methyl-2H-1,4-benzodiazepin-2-one as a colourless oil.

WORKUP

后处理

  1. additionadd (10 ml)
  2. customA white solid precipitated which
  3. filtrationwas filtered off
  4. additionThe solid was treated with 10% sodium hydroxide solution (50 ml)
  5. extractionextracted with ethyl acetate (80 ml)
  6. customThe organic layer was separated
  7. dry with materialdried (Na2SO4)
  8. customevaporated