反应详情

温度

0 °C

A solution of 10 (28.62 g, 75 mmol) in tetrahydrofuran (375 mL) containing acetic acid (4.5 g, 75 mmol) was treated at 0° C. with 1 M tetrabutylammonium fluoride (75 mL, 75 mmol) and the mixture was stirred at 0° C. for 40 min. The solvent was evaporated and the residue was dissolved in diethyl ether (250 mL) and washed with saturated aq. sodium bicarbonate and brine, dried and evaporated to give a brown solid which was washed with cold hexanes to give 11 as white fluffy needles (14.13 g, 70%), mp 118-120° C. (from dichloromethane-hexanes), (lit.11 mp 121-124° C.).

1. customThe solvent was evaporated
2. dissolutionthe residue was dissolved in diethyl ether (250 mL)
3. washwashed with saturated aq. sodium bicarbonate and brine
4. customdried
5. customevaporated
6. customto give a brown solid which
7. washwas washed with cold hexanes