反应详情

温度

-20 °C

2-(4-Hydroxyphenyl)ethanol(356 g, 2.58 mol, 1.0 eq) was dissolved in methylene chloride (3500 ml) and triethyl amine (653 g, 6.44 mol, 2.5 eq). The mixture was cooled to −20° C. Methanesulfonyl chloride (657 g, 5.74 mol. 2.2 eq) was then added keeping the temperature between −25° C. and −15° C. When the conversion was >95% salts were formed which were filtered off and washed with methylene chloride (600 ml). The organic layer was washed first with saturated sodium hydrogencarbonate solution (700 ml) at 20° C. followed by water (700 ml). The methylene chloride was evaporated to dryness and the remaining residue was then used in the subsequent step.

1. customthe temperature between −25° C. and −15° C
2. customwere formed which
3. filtrationwere filtered off
4. washwashed with methylene chloride (600 ml)
5. washThe organic layer was washed first with saturated sodium hydrogencarbonate solution (700 ml) at 20° C.
6. customThe methylene chloride was evaporated to dryness