反应详情

To a solution of 3.87 g piperidine-3-carboxylic acid ethyl ester hydrochloride (commercially available) (20 mmol) in 40 mL DCM was added 10 mL of DIPEA (60 mmol). At room temperature 2.72 mL 2-chloro-benzenesulfonyl chloride (20 mmol) was added drop wise and stirred for 14 h. The mixture was diluted with 30 mL of DCM, washed with water (3×50 mL) and the organic layer was dried over anhydrous sodium sulfate, filtered and evaporated under reduced pressure to obtain the crude product which was further purified by column chromatography on silica eluting with 10% ethyl acetate in hexane to yield 5.73 g (86.3%) of the title compound. (MH+) 332.16.

1. washwashed with water (3×50 mL)
2. dry with materialthe organic layer was dried over anhydrous sodium sulfate
3. filtrationfiltered
4. customevaporated under reduced pressure
5. customto obtain the crude product which
6. customwas further purified by column chromatography on silica eluting with 10% ethyl acetate in hexane