HRID436130

反应详情

EQUATION

反应方程式

HRID 436130 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 0.5 g. of 1,3,4,9-tetrahydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one and 0.5 g. of sulfur is fused at 160° C. ± 5 for 1 hour. The fusion mixture is slurried with chloroform and filtered. The filtrate is chromatographed on silica gel with benzene:methanol 9:1 to give a solid, which is recrystallized from methanol-water to give a tan solid, m.p. 224°-225° C. (dec.).

WORKUP

后处理

  1. additionA mixture of 0.5 g
  2. filtrationfiltered
  3. customThe filtrate is chromatographed on silica gel with benzene:methanol 9:1
  4. customto give a solid, which
  5. customis recrystallized from methanol-water
  6. customto give a tan solid, m.p. 224°-225° C. (dec.)