反应详情

3-Chloroperoxybenzoic acid (195 mg) was added to a 0° C. suspension of the compound prepared in Example 93 (100 mg) in dichloromethane (4 mL). The reaction was stirred one hour at room temperature. Diisopropylethylamine (0.669 mL) and the compound prepared in Example 9 (198 mg) were added and the mixture was stirred at room temperature for 18 hours. The reaction was diluted with ethyl acetate and sequentially washed with a saturated sodium bicarbonate solution and brine. The organics were dried over magnesium sulfate and concentrated. The residue was purified by column chromatography on silica gel (concentrated aqueous ammonia:methanol:ethyl acetate=0.1:0.9:25) to obtain the title compound (51 mg) having the following physical data.

1. stirringthe mixture was stirred at room temperature for 18 hours
2. washsequentially washed with a saturated sodium bicarbonate solution and brine
3. dry with materialThe organics were dried over magnesium sulfate
4. concentrationconcentrated
5. customThe residue was purified by column chromatography on silica gel (concentrated aqueous ammonia:methanol:ethyl acetate=0.1:0.9:25)