反应详情

温度

60 °C

A solution of 120.50 g of ethyl 6-oxaspiro[2.5]-octane-1-carboxylate in 700 ml of ethanol/water 3.5:1 is mixed with 55.20 g of potassium hydroxide. The reaction mixture is heated at 60° C. for 4 hours, the ethanol is distilled off and the aqueous residue is diluted with water and extracted with tert-butyl methyl ether. The aqueous phase is adjusted to pH 2 with 4M hydrochloric acid and extracted with tert-butyl methyl ether. The combined organic extracts are washed with brine, dried with sodium sulphate and evaporated. The title compound is obtained as a yellowish oil and is employed without further purification for the next stage. Rt=2.13 (Gradient I).

1. distillationthe ethanol is distilled off
2. additionthe aqueous residue is diluted with water
3. extractionextracted with tert-butyl methyl ether
4. extractionextracted with tert-butyl methyl ether
5. washThe combined organic extracts are washed with brine
6. dry with materialdried with sodium sulphate
7. customevaporated