反应详情

温度

80 °C

Add to a solution of ditert-butyl(1R,2S,4R,5R,6R)-4-bromo-2-(tert-butoxycarbonylamino)bicyclo[3.1.0]hexane-2,6-dicarboxylate (2 g, 4.20 mmol) in dimethylformamide (10 mL), 1H-1,2,4-triazole-3-thiol (525 mg, 5.04 mmol) and potassium carbonate (1.16 g, 8.4 mmol). Stir the mixture at 80° C. overnight. Cool to room temperature and dilute with ethyl acetate, wash with 10% citric acid and brine, dry over anhydrous sodium sulfate, filter and concentrate to dryness. Purify by silica gel chromatography (80 g silica column) eluting with hexane:ethyl acetate (80:20 to 0:100) to obtain the title compound (1.64 g, 78%). MS (m/z): 497 (M+1).

1. temperatureCool to room temperature
2. washwash with 10% citric acid and brine
3. dry with materialdry over anhydrous sodium sulfate
4. filtrationfilter
5. concentrationconcentrate to dryness
6. customPurify by silica gel chromatography (80 g silica column)
7. washeluting with hexane:ethyl acetate (80:20 to 0:100)