反应详情

A mixture of 20.2 g of 4-tert.butyl-cyclohexane-1-carboxaldehyde, 52 g of (α-carbethoxy-ethylidene)-triphenyl-phosphorane and 3.6 g of benzoic acid in 120 ml of toluene is heated at reflux for 16 hours under nitrogen gasification and the toluene is evaported. The oily-crystalline residue is dissolved in 600 ml of methanol/water (4:1) and exhaustively extracted with hexane. The combined hexane extracts are washed with sodium bicarbonate solution and water, dried over sodium sulphate and evaporated. By distillation there is obtained pure 3-(4-tert.butyl-cyclohexyl)-2-methyl-acrylic acid ethyl ester of boiling point 99° C./0.03 Torr.

1. temperatureis heated
2. temperatureat reflux for 16 hours under nitrogen gasification
3. extractionexhaustively extracted with hexane
4. washThe combined hexane extracts are washed with sodium bicarbonate solution and water
5. dry with materialdried over sodium sulphate
6. customevaporated
7. distillationBy distillation there