反应详情

温度

0 °C

The methyl 4-methyl-3-phenyl-4-pentenoate (258.3 g, 1.251 mol) was added, at 0° C. under nitrogen, to lithium aluminum hydride (25 g, 0.625 mol) in dry THF (1 liter), drop-wise. After 30 minutes, the cooling bath was removed and the reaction allowed reaching room temperature. After 24 h, more THF (1 liter) was added and the reaction was cooled to 0° C. and treated successively with water (25 ml), 5% aqueous sodium hydroxide (75 ml) and water (25 ml). The reaction was stirred at room temperature for 30 minutes. Anhydrous solid sodium sulfate was added (100 g) and stirring continued for 5 minutes The solid was filtered off, rinsed with diethyl ether and the filtrate was evaporated under vacuum. The product was purified distillation through a 20-cm Widmer column. 214 g of the desired product were obtained (yield=97%).

1. customthe cooling bath was removed
2. customallowed reaching room temperature
3. waitAfter 24 h
4. additionmore THF (1 liter) was added
5. additiontreated successively with water (25 ml), 5% aqueous sodium hydroxide (75 ml) and water (25 ml)
6. additionAnhydrous solid sodium sulfate was added (100 g)
7. stirringstirring
8. waitcontinued for 5 minutes
9. filtrationThe solid was filtered off
10. washrinsed with diethyl ether
11. customthe filtrate was evaporated under vacuum
12. customThe product was purified
13. distillationdistillation through a 20-cm Widmer column