反应详情

To a stirred suspension of 1.5 g (0.04 mole) of lithium aluminium hydride and 75 ml of dried diethyl ether are added over 1/2 hour 15 g (0.08 moles) of 2-methyl-4-(2,2,3-trimethylcyclopent-1-yl)-but-2-enal. The mixture is heated under argon to reflux for 2 hours. It is cooled with ice water and, with caution, treated first with water until hydrogen no longer evolves and then with HCl 5%, whereupon the aluminium hydroxide precipitate dissolves. The material is extracted with ether and the combined organic phases are washed with saturated common salt; it is then dried over MgSO4 and distilled. A fractional vacuum distillation leads to 8.3 g of 2-methyl-4-(2,2,3-trimethyl-cyclopent-1-yl)-but-2-en-1-ol (mixture of isomers) (55% yield);

1. temperatureThe mixture is heated under argon
2. temperatureto reflux for 2 hours
3. extractionThe material is extracted with ether
4. washthe combined organic phases are washed with saturated common salt
5. dry with materialit is then dried over MgSO4
6. distillationdistilled
7. distillationA fractional vacuum distillation