反应详情

Add to a solution of 4-benzyloxycarbonyl-piperazin-2-one (2 g, 8.6 mmol) in dry THF (10 mL/mmol) under nitrogen, sodium hydride (236 mg, 9.4 mmol, 60% dispersion in mineral oil) in one portion and stir at room temperature for 30 min. Add p-methoxybenzyl chloride (1.86 mL, 13 mmol) and stir at room temperature overnight. Concentrate, add ethyl acetate, wash with water, saturated aqueous sodium chloride, dry (magnesium sulfate), concentrate and purify (silica gel chromatography, eluting with 1:1 hexanes:ethyl acetate) to give the title compound as an oil (1.6 g, 54%).

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