HRID436130
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionA mixture of 0.5 g
- filtrationfiltered
- customThe filtrate is chromatographed on silica gel with benzene:methanol 9:1
- customto give a solid, which
- customis recrystallized from methanol-water
- customto give a tan solid, m.p. 224°-225° C. (dec.)