HRID223392
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
2.533 gm (0.01 mol) of 3-acetyl-5,6-dimethoxy-2(3H)-benzothiazolone were refluxed for 2 hours in a mixture of 40 ml of ethanol and 50 ml of concentrated ammonia. The mixture was concentrated to one-fourth of its original volume, allowed to cool and filtered. The dried residue was purified by chromatography on silica gel, using 1,2-dichloroethane/acetone (volume ratio 9:1) for elution. The residues of the evaporated eluates were recrystallized from methanol in the presence of activated charcoal, yielding 1.78 gm (84% of theory) of the desired product having a melting point of 192°-193° C.
WORKUP
后处理
- concentrationThe mixture was concentrated to one-fourth of its original volume
- temperatureto cool
- filtrationfiltered
- customThe dried residue was purified by chromatography on silica gel
- washfor elution
- customThe residues of the evaporated eluates were recrystallized from methanol in the presence of activated charcoal