HRID26503

反应详情

EQUATION

反应方程式

HRID 26503 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 1.83 g of 11H-s-triazolo[3,4-b][3]benzazepine in 40 ml of chloroform was added 0.1 ml of pyridine and 0.55 ml of bromine was added dropwise under stirring. The mixture was stirred for 2 hours, after which it was washed with water and dried over Na2SO4. After evaporation of the solvent, the residue was treated with ether. By the above procedure was obtained 3-bromo-11H-s-triazolo[3,4-b][3]benzazepine as crystals. These crystals were recrystallized from ethanol and methanol in the order mentioned to obtain pale-brown platelets melting at 169°-170° C.

WORKUP

后处理

  1. additionwas added dropwise
  2. stirringThe mixture was stirred for 2 hours
  3. washafter which it was washed with water
  4. dry with materialdried over Na2SO4
  5. customAfter evaporation of the solvent
  6. additionthe residue was treated with ether