反应详情

To a solution of (R)-tert-butyl 2-(hydroxymethyl)morpholine-4-carboxylate (1 g) in dichloromethane (50 mL) was added triethylamine (1.604 mL) and 4-methylbenzene-1-sulfonyl chloride (1.097 g). The mixture was stirred at ambient temperature under nitrogen for 72 hours. The reaction was diluted with methylene chloride (50 mL) and brine (100 mL). The brine layer was extracted with methylene chloride (75 mL). The combined organics were dried over sodium sulfate, filtered and concentrated. The crude material was purified on a silica gel column eluting with a 15-65% ethyl acetate in hexane gradient to give the title compound.

1. extractionThe brine layer was extracted with methylene chloride (75 mL)
2. dry with materialThe combined organics were dried over sodium sulfate
3. filtrationfiltered
4. concentrationconcentrated
5. customThe crude material was purified on a silica gel column
6. washeluting with a 15-65% ethyl acetate in hexane gradient