反应详情

A mixture of trans-tert-butyl 4-fluoro-3-hydroxypiperidine-1-carboxylate (3.10 g, 14.1 mmol) and 4-methylbenzene-1-sulfonyl chloride (5.39 g, 28.3 mmol) in pyridine (20 mL) was stirred at room temperature for 18 hours. The pyridine was removed in vacuo, and the residue was dissolved in ethyl acetate (30 mL), washed with brine, dried (sodium sulfate) and concentrated in vacuo. The residue obtained was purified by flash chromatography on silica gel (hexane:ethyl acetate 2:1) to give trans-tert-butyl 4-fluoro-3-(tosyloxy)piperidine-1-carboxylate (3.95 g, 75%) as a solid.

1. customThe pyridine was removed in vacuo
2. dissolutionthe residue was dissolved in ethyl acetate (30 mL)
3. washwashed with brine
4. dry with materialdried (sodium sulfate)
5. concentrationconcentrated in vacuo
6. customThe residue obtained
7. customwas purified by flash chromatography on silica gel (hexane:ethyl acetate 2:1)