反应详情

13.10 g (32 mmol) of 9H-fluoren-9-ylmethyl[4-(2-methyl-[1,3]dioxolan-2-yl)cyclohexyl]carbamate (cis/trans mixture) and 1.30 g of p-toluenesulfonic acid are refluxed in 25 mL of water and 500 mL of acetone for 16 hours with stirring. Then the reaction mixture is concentrated by evaporation and the residue is dissolved in ethyl acetate and extracted with water. The organic phase is dried and evaporated to dryness. The residue is extracted with diisopropylether and suction filtered. Yield: 7.77 g (89%) of cis compound; NMR: LH201628.

1. concentrationThen the reaction mixture is concentrated by evaporation
2. dissolutionthe residue is dissolved in ethyl acetate
3. extractionextracted with water
4. customThe organic phase is dried
5. customevaporated to dryness
6. extractionThe residue is extracted with diisopropylether and suction
7. filtrationfiltered