反应详情

A room temperature solution of Example 73A (145 mg,0.44 mmol) in 1:1 TFA/dichloromethane (10 mL) was stirred for 4 hours and concentrated. The concentrate was dissolved in ethanol (2 mL), treated with 3,4-dihydro-1(2H)-naphthalenone (8.2 mg, 0.06 mmol) and pyridinium p-toluenesulfonate (2 mg, 0.008 mmol), heated to reflux, stirred for 2 hours, cooled to room temperature, and concentrated. The concentrate was purified by flash column chromatography on silica gel with 4% methanol/dichloromethane to provide the desired product. MS (ESI(−)) m/e 359 (M−H)−.

1. concentrationconcentrated
2. dissolutionThe concentrate was dissolved in ethanol (2 mL)
3. temperatureheated
4. temperatureto reflux
5. concentrationconcentrated
6. customThe concentrate was purified by flash column chromatography on silica gel with 4% methanol/dichloromethane