反应详情

Potassium tert-butoxide (1M in THF, 1.95 ml) is added to cyclopropylcarboxamide oxime (0.195 g) in THF (7 ml) at 0°. After 10 min ethyl 4,5-dihydro-4,4-dimethylimidazo[1,5-a]quinoxaline-3-carboxylate (XXXIII, EXAMPLE 94, 0.503 g) is added. The ice bath is removed after stirring for 10 min and the reaction is allowed to slowly warm to 20°-25°. After 2 hr DMF (4 ml) is added. When the reaction had stirred for a total of 7 hr, the solvents are removed under reduced pressure and the residue is partitioned between ethyl acetate and saline. The phases are separated, the organic phase is dried over magnesium sulfate and concentrated to give the title compound; mp 175°-179°; NMR (CDCl3): 1.10, 1.76, 2.18, 3.83, 6.79, 6.85, 7.13, 7.42 and 8.10 δ.

1. customThe ice bath is removed
2. temperatureto slowly warm to 20°-25°
3. additionAfter 2 hr DMF (4 ml) is added
4. stirringWhen the reaction had stirred for a total of 7 hr
5. customthe solvents are removed under reduced pressure
6. customthe residue is partitioned between ethyl acetate and saline
7. customThe phases are separated
8. dry with materialthe organic phase is dried over magnesium sulfate
9. concentrationconcentrated