反应详情

Sodium (0.48 g, 21 mmol) was reacted with anhydrous benzyl alcohol (20 ml) under nitrogen at room temperature. The mixture was then cooled in an ice bath and (71) (3.22 g, 10 mmol) was added. After 1 hr., the mixture was stirred at room temperature for overnight. The mixture was evaporated in vacuo and the residue was dissolved in ether, washed with water, dried with anhydrous magnesium sulfate, filtered, and evaporated in vacuo. The residue was purified by silica gel column chromatography (eluent, ether:hexanes (1:9)) to afford 3.18 g (68%) of a colorless syrup. 1H NMR (200 MHz, CDCl3) δ 1.28 (6H, d, J=7.2 Hz), 2.39 (3H, s), 3.40 (1H, m), 5.14 (2H, s), 5.42 (2H, s), 7.13-7.44 (13H, m).

1. temperatureThe mixture was then cooled in an ice bath
2. customThe mixture was evaporated in vacuo
3. dissolutionthe residue was dissolved in ether
4. washwashed with water
5. dry with materialdried with anhydrous magnesium sulfate
6. filtrationfiltered
7. customevaporated in vacuo
8. customThe residue was purified by silica gel column chromatography (eluent, ether:hexanes (1:9))