反应详情

A mixture of 46.3 g of 4-tert.amyl-cyclohexane-1-carboxaldehyde, 92.3 g of (α-carbethoxy-ethylidene)-triphenyl-phosphorane and 7.6 g of benzoic acid in 250 ml of toluene is heated at reflux for 3.5 hours under nirogen gasification and the toluene is evaporated. The oily-crystalline residue is dissolved in 1600 ml of methanol/water (4:1) and exhaustively extracted with hexane. The combined hexane extracts are washed with sodium carbonate solution and water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 3-(4-tert.amyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester of boiling point 113°-115° C./0.03 Torr.

1. temperatureis heated
2. temperatureat reflux for 3.5 hours under nirogen gasification
3. customthe toluene is evaporated
4. dissolutionThe oily-crystalline residue is dissolved in 1600 ml of methanol/water (4:1)
5. extractionexhaustively extracted with hexane
6. washThe combined hexane extracts are washed with sodium carbonate solution and water
7. dry with materialdried over sodium sulphate
8. customevaporated
9. distillationBy distillation there