反应详情

Toluene sulphonyl chloride (0.513 g, 2.69 mmol) was added to a solution of (S)-tert-butyl 2-(hydroxymethyl)morpholine-4-carboxylate (0.390 g, 1.79 mmol), triethylamine (0.50 mL, 3.59 mmol) and DMAP (cat.) in dichloromethane (11 mL). The reaction mixture was stirred for 24 h then diluted with dichloromethane (25 ml) and washed sequentially with water (25 mL) and 0.2M HCl (25 mL). The organic phase was dried (Na2SO4) and the solvent was removed in vacuo. The crude product was purified by flash column chromatography on silica gel, eluting with ethyl acetate/hexane (1/5), to give the title compound as a colourless solid (0.650 g, 97%).

1. washwashed sequentially with water (25 mL) and 0.2M HCl (25 mL)
2. dry with materialThe organic phase was dried (Na2SO4)
3. customthe solvent was removed in vacuo
4. customThe crude product was purified by flash column chromatography on silica gel
5. washeluting with ethyl acetate/hexane (1/5)