反应详情

A mixture of the compound (70 mg) obtained in Example 30, 2N methylamine in tetrahydrofuran solution (0.65 ml), triethylamine (59 mg), bis(2-oxo-3-oxazolidinyl)phosphinoyl chloride (39 mg) and methylene chloride (5 ml) was stirred overnight at room temperature. The reaction mixture was diluted with ethyl acetate, washed with water and saturated brine, dried over anhydrous sodium sulfate, and concentrated is under reduced pressure. The residue was purified by column chromatography [developing solvent:ethyl acetate-methanol (10:1, volume ratio)] and recrystallized from ethyl acetate-hexane (1:1, volume ratio) to give the title compound (14 mg) as a colorless powder.

1. washwashed with water and saturated brine
2. dry with materialdried over anhydrous sodium sulfate
3. concentrationconcentrated
4. customThe residue was purified by column chromatography [developing solvent:ethyl acetate-methanol (10:1, volume ratio)]
5. customrecrystallized from ethyl acetate-hexane (1:1, volume ratio)