反应详情

To a mixture of the compound of Example 77 (200 mg, 0.423 mmol) and THF (10 mL) was added ethyl isocyanate (101 μL, 1.27 mmol) at 0° C., and the mixture was stirred at room temperature for 15 hr. The reaction mixture was diluted with ethyl acetate, washed with water and saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was purified by aminosilica gel chromatography (eluate; ethyl acetate). Recrystallization of the obtained solid from ethyl acetate-THF gave the title compound (172 mg, 75%) as a white powder.

1. washwashed with water and saturated brine
2. dry with materialdried over magnesium sulfate
3. concentrationconcentrated under reduced pressure
4. customThe residue was purified by aminosilica gel chromatography (eluate; ethyl acetate)
5. customRecrystallization of the obtained solid from ethyl acetate-THF