HRID2419570
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 slurry of 3-[(1,3-benzodithiol-2-ylidene)amino]-2 -thioxo-4-thiazolidinone (see example 37), m-trifluoromethylbenzaldehyde (10 ml, excess) and acetic acid/piperidine (1 ml) in 250 ml of anhydrous glyme is heated at reflux for seven days. The reaction mixture is concentrated in vacuo and the oily residue extracted with hexane. The solid thus obtained is slurried in 1000 ml of dichloromethane and stirred at room temperature overnight. The slurry is filtered and the filtrate concentrated in vacuo. The solid residue thus obtained is recrystallized from dimethylformamide to yield 500 mg of the title compound, melting point 268°-269° C.
WORKUP
后处理
- temperatureat reflux for seven days
- concentrationThe reaction mixture is concentrated in vacuo
- extractionthe oily residue extracted with hexane
- customThe solid thus obtained
- filtrationThe slurry is filtered
- concentrationthe filtrate concentrated in vacuo
- customThe solid residue thus obtained
- customis recrystallized from dimethylformamide