反应详情

The compound prepared in Example 406 (0.533 g), benzotriazole-1-yl-oxy-tris-(dimethylamino)-phosphonium hexafluorophosphate (2.0098 g), the compound prepared in Example 214 (1.3315 g) and triethyl amine were suspended in dimethyl formamide (40 mL) and stirred at room temperature overnight. The reaction mixture was poured onto saturated aqueous sodium bicarbonate and ethyl acetate. The organics were washed with brine, dried over with magnesium sulfate and concentrated under reduced pressure to afford the crude material. The crude material was purified by flash column chromatography (eluant gradient elution 1-5% (9:1=methanol:ammonium hydroxide)/ethyl acetate) to furnish the title compound (0.902 g), possessing the following physical data.

1. washThe organics were washed with brine
2. dry with materialdried over with magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. customto afford the crude material
5. customThe crude material was purified by flash column chromatography (eluant gradient elution 1-5% (9:1=methanol:ammonium hydroxide)/ethyl acetate)