反应详情

Acetyl chloride (0.36 ml) is added to 1,2,3,4-tetrahydroquinoxalin-2-one (IV, EXAMPLE 1, 0.676 g) and triethylamine (0.76 ml) in THF (8 ml) at 0°. After stirring for 1 hr, the solvent is removed under reduced pressure and the residue is partitioned between dichloromethane and aq. sodium bicarbonate. The layers are separated, the organic phase is filtered through sodium sulfate and concentrated. The concentrate is crystallized from methanomethylene chloride/hexane to give the title compound, mp 164°-165°; NMR (CDCl3) 2.28, 4.54, 7.00, 7.11, 7.21 and 9.19 δ.

1. customthe solvent is removed under reduced pressure
2. customthe residue is partitioned between dichloromethane and aq. sodium bicarbonate
3. customThe layers are separated
4. filtrationthe organic phase is filtered through sodium sulfate
5. concentrationconcentrated
6. customThe concentrate is crystallized from methanomethylene chloride/hexane