反应详情

温度

40 °C

46 g. of a 70% sodium dihydro-bis(2-methoxyethoxy)-aluminate solution in toluene are added dropwise at 25°-30° C. over a period of 90 minutes to a solution of 25.3 g of 3-(4-tert.butyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester in 130 ml of absolute toluene and the mixture is subsequently warmed at 40° C. for 2 hours. The mixture is then cooled down to -10° C., treated dropwise with 130 ml of 2-N sodium hydroxide, the toluene phase is separated and the aqueous-alkaline phase is back-extracted twice with 200 ml of toluene. The combined toluene phases are washed neutral with water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 3-(4-tert.butyl-cyclohexyl)-2-methyl-allyl alcohol of boiling point 112°-114° C./0.08 Torr.

1. temperatureThe mixture is then cooled down to -10° C.
2. customthe toluene phase is separated
3. extractionthe aqueous-alkaline phase is back-extracted twice with 200 ml of toluene
4. washThe combined toluene phases are washed neutral with water
5. dry with materialdried over sodium sulphate
6. customevaporated
7. distillationBy distillation there