反应详情

N-(1-(tert-butoxycarbonyl)sulfamoyl)pyridine-4(1H)-ylidene)-N-methylmethanaminium (A) (5.81 g, 19.32 mmol) was added to a suspension of ethyl 2-(4-(aminomethyl)phenyl)propanoate (4.0 g, 19.32 mmol) in dichloromethane (40 mL) at room temperature and stirred for 16 h. The reaction mixture was diluted with water (100 mL) and extracted with ethyl acetate (2×75 mL). Combined organic layer was washed with water (50 mL), brine (50 mL), dried over sodium sulfate and concentrated to get crude compound, which was purified by column chromatography (silica gel; 100-200 mesh). The product eluted with 20% ethyl acetate in pet ether to yielded ethyl 2-(4-((N-(tert-butoxycarbonyl)sulfamoylamino)methyl)phenyl)propanoate (3.8 g, 51%) as pale yellow solid.

1. extractionextracted with ethyl acetate (2×75 mL)
2. washCombined organic layer was washed with water (50 mL), brine (50 mL)
3. dry with materialdried over sodium sulfate
4. concentrationconcentrated
5. customto get crude compound, which
6. customwas purified by column chromatography (silica gel; 100-200 mesh)
7. washThe product eluted with 20% ethyl acetate in pet ether