反应详情

温度

0 °C

Place a mixture of α-[(trimethylsilyl)ethynyl]-benzene-methanol (4.09 g, 20 mmol) and tetrahydrofuran (25 mL) under argon atmosphere and cool to 0° C. Add, by dropwise addition, tetra-n-butylammonium fluoride (25 mL of a 1M solution in tetrahydrofuran, 25 mmol). Allow to warm to room temperature and stir for 1 hour. Partition between ethyl ether and water. Separate the organic phase, wash with saturated aqueous sodium chloride and concentrate in vacuo. Purify by silica gel chromatography (15% ethyl acetate/hexane) then purify further by distillation to yield 2.15 g of the title compound; bp 100°-110° C. @0.1 mm Hg.

1. temperatureAllow to warm to room temperature
2. customPartition between ethyl ether and water
3. customSeparate the organic phase
4. washwash with saturated aqueous sodium chloride
5. concentrationconcentrate in vacuo
6. customPurify by silica gel chromatography (15% ethyl acetate/hexane)
7. distillationthen purify further by distillation