反应详情

To a stirred solution of 5-hydroxy-2-benzothiazolesulfonamide 1.15 g., 0.005 mole) triethylamine (0.7 ml, 0.005 mole) and 4-dimethylaminopyridine (5 mg, catalyst) in dimethylformamide (10 ml) is added 2-(4-chlorophenyl)acetyl chloride (0.8 ml). The reaction mixture is stirred for 2 hours, poured into ice water, acidified with hydrochloric acid and extracted with ether. The organic extract is washed with water and dried over magnesium sulfate. The ether is distilled at reduced pressure and the residue chromatographed on silica gel as eluant (130 g, 70-230 mesh) using ethylacetatehexane (1:1) to give 2-sulfamoyl-5-benzothiazolyl 2-(4-chlorophenyl)acetate.

1. extractionextracted with ether
2. extractionThe organic extract
3. washis washed with water
4. dry with materialdried over magnesium sulfate
5. distillationThe ether is distilled at reduced pressure
6. customthe residue chromatographed on silica gel as eluant (130 g, 70-230 mesh)