反应详情

To a stirring solution of 2-(4-oxanyl)ethanol (9.63 g, 74.0 mmol) in dry dichloromethane (350 mL) was added distilled triethylamine (20.62 mL, 96.2 mmol) at 0° C., followed by drop-wise addition of methanesulfonyl chloride (7.44 mL, 96.2 mmol) over 15 min. The reaction was stirred for 16 h under N2 and slowly allowed to come to ambient temperature. The reaction was washed with saturated NaHCO3 (100 mL) and the aqueous phase was extracted with dichloromethane (1×50 mL). The combined organic extracts were dried (K2CO3), filtered and concentrated by rotary evaporation to yield 11.9 g of a colorless oil (77.0% yield).

1. customto come to ambient temperature
2. washThe reaction was washed with saturated NaHCO3 (100 mL)
3. extractionthe aqueous phase was extracted with dichloromethane (1×50 mL)
4. dry with materialThe combined organic extracts were dried (K2CO3)
5. filtrationfiltered
6. concentrationconcentrated by rotary evaporation