反应详情

5.0 g of known monoethyl 1,1-cyclopropanedicarboxylate, 4.5 ml of triethylamine and 6.9 ml of diphenyl phosphorazidate (DPPA) were added to 80 ml of tert-butyl alcohol and the mixture was refluxed at 90° to 100° C. for 4 h. After distilling the solvent, the residue was dissolved in ethyl acetate and washed with 5% citric acid, saturated aqueous sodium carbonate solution and saturated aqueous sodium chloride solution and then dried. The solvent was distilled off to obtain 5.7 g of the desired compound (P-12) in the form of a light yellow oil.

1. temperaturethe mixture was refluxed at 90° to 100° C. for 4 h
2. distillationAfter distilling the solvent
3. dissolutionthe residue was dissolved in ethyl acetate
4. washwashed with 5% citric acid, saturated aqueous sodium carbonate solution and saturated aqueous sodium chloride solution
5. customdried
6. distillationThe solvent was distilled off