反应详情

温度

60 °C

Add 2.5M sodium hydroxide (15.55 mL, 38.88 mmol) to a stirred solution of the ditert-butyl (1S,2S,5R,6R)-2-(tert-butoxycarbonylamino)-4-oxo-bicyclo[3.1.0]hexane-2,6-dicarboxylate (2.0 g, 4.86 mmol) in tetrahydrofuran (24.3 mL) and ethanol (9.72 mL). Heat the reaction mixture to 60° C. and maintain stirring overnight. Continue heating for 4 hours then wash with ethyl acetate. Cool the aqueous phase in an ice bath and acidify to pH=2-3 with 1N hydrochloric acid solution. Extract with ethyl acetate (3 times), dry the organic on sodium sulfate, filter and concentrate to give the title compound as an orange solid (1.4 g, 96%). MS (m/z): 322 (M+23).

1. temperaturemaintain
2. temperatureContinue heating for 4 hours
3. washthen wash with ethyl acetate
4. temperatureCool the aqueous phase in an ice bath
5. extractionExtract with ethyl acetate (3 times)
6. customdry the organic on sodium sulfate
7. filtrationfilter
8. concentrationconcentrate