反应详情

Dissolve 4-benzyloxycarbonylpiperazin-2-one (2 g, 8.6 mmol) in THF (10 mL). Add sodium hydride (236 mg, 9.4 mmol, 60% dispersion in mineral oil) in one portion and stir at room temperature for 30 min. Add iodomethane (0.8 mL, 13 mmol) and stir at room temperature overnight. Concentrate, add ethyl acetate and wash with water. Separate organic layer, wash with saturated aqueous sodium chloride, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with ethyl acetate) to give the title compound as a yellow oil (1.7 g, 82%).

1. concentrationConcentrate
2. additionadd ethyl acetate
3. washwash with water
4. washSeparate organic layer, wash with saturated aqueous sodium chloride
5. dry with materialdry (magnesium sulfate)
6. concentrationconcentrate
7. custompurify
8. wash(silica gel chromatography, eluting with ethyl acetate)