HRID354739

反应详情

EQUATION

反应方程式

HRID 354739 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.5 g (0.0044 mol) of 5-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-7-nitro-2H-1,4-benzodiazepin-2-one are dissolved in 15 ml of concentrated hydrochloric acid, treated with 3.3 g of tin (II) chloride and stirred at room temperature for 15 minutes. The reaction mixture is poured into a mixture of ice and soda solution and extracted with methylene chloride. After drying and evaporating the organic phase, the residue is recrystallised from ether. There is obtained 7-amino-5-(o-fluorophenyl)-1,3-dihydro-1,3,3-trimethyl-2H-1,4-benzodiazepin-2-one of melting point 190°-191°.

WORKUP

后处理

  1. additionThe reaction mixture is poured into a mixture of ice and soda solution
  2. extractionextracted with methylene chloride
  3. customAfter drying
  4. customevaporating the organic phase
  5. customthe residue is recrystallised from ether