反应详情

To a suspension of 0.83 g (S)-4-benzylcarbamoyl-2-tert-butoxycarbonylamino-butyric acid benzyl ester and 1.28 g triphenylphosphine in 16 ml acetonitrile were added dropwise at 0° C. 1.00 ml diisopropylazodicarboxylate and after 2 minutes 0.67 ml trimethylsilylazide over a period of 10 minutes. After 30 minutes the mixture was allowed to warm to RT and stirred for 12 h. The mixture was cooled to 0° C. and 0.67 ml aqueous sodium nitrite (2.9 M) were added, after 30 minutes a solution of 1.07 g ceric ammonium nitrate in 10 ml water was added and stirred for another 20 minutes. After this time the mixture was poured into ice and extracted twice with dichloromethane.

1. additionwere added dropwise at 0° C
2. temperatureThe mixture was cooled to 0° C.
3. additionwas added
4. stirringstirred for another 20 minutes
5. additionAfter this time the mixture was poured into ice
6. extractionextracted twice with dichloromethane