反应详情

A solution of Example 1D (212 mg, 0.49 mmol) and tert-butylcarbazate (976 mg, 2.3 mmol) in ethanol (5 mL) was heated to reflux, stirred for 16 hours, diluted with ethyl acetate (50 mL), washed with water and brine, dried (MgSO4), filtered, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 1:0.5:98.5/methanol:acetic acid:dichloromethane, then 2:0.5:97.5/methanol:acetic acid:dichloromethane to provide the desired product. MS (ESI(−)) m/e 331 (M−H)−.

1. temperatureto reflux
2. washwashed with water and brine
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. customThe concentrate was purified by flash column chromatography on silica gel with 1:0.5:98.5/methanol