反应详情

Triethylamine (13.9 mmol, 2.0 equiv.) was added at 0° C. to a solution of methyl 1-aminocyclobutanecarboxylate (6.97 mmol, 1 equiv.) in dichloromethane p.a. (20 ml), and the mixture was stirred for 10 minutes. 4-Methoxy-2,6-dimethyl-phenylsulfonyl chloride (8.36 mmol, 1.2 equiv.), dissolved in DCM (5 ml), was slowly added dropwise at the same temperature, and the mixture was stirred for 4 hours at 25° C. The reaction mixture was diluted with dichloromethane (100 ml), washed with distilled water (2×50 ml) and saturated sodium chloride solution (2×50 ml) and dried over sodium sulfate. The solvent was concentrated and the crude product was purified by column chromatography (15% ethyl acetate in hexane) to yield the desired product in the form of a white solid. Yield: 66%

1. additionwas slowly added dropwise at the same temperature
2. stirringthe mixture was stirred for 4 hours at 25° C
3. washwashed with distilled water (2×50 ml) and saturated sodium chloride solution (2×50 ml)
4. dry with materialdried over sodium sulfate
5. concentrationThe solvent was concentrated
6. customthe crude product was purified by column chromatography (15% ethyl acetate in hexane)