反应详情

To a stirred solution of (E)-methyl 4-bromo-2-(4-chloro-5H-1,2,3-dithiazol-5-ylideneamino)benzoate (100 mg, 0.27 mmol, 1 eq) in THF was added butane-1,4-diamine (0.027 mL, 0.27 mmol, 1 eq) dropwise under N2 and the reaction was heated at reflux for 3 hours. After it was cooled to rt, the reaction mixture was diluted with water (20 mL) and extracted with ethyl acetate (3×20 mL). The combined organic layers were dried over Na2SO4 and concentrated under reduced pressure to give the desired product, which was purified by silica gel chromatography. MS (ESI): 294, 296 (MH+).

1. temperaturethe reaction was heated
2. temperatureat reflux for 3 hours
3. extractionextracted with ethyl acetate (3×20 mL)
4. dry with materialThe combined organic layers were dried over Na2SO4
5. concentrationconcentrated under reduced pressure