反应详情

A solution of 1-amino-indoline hydrochloride (1.0 g) and 2,4-dioxopiperidine (663 mg) in absolute ethanol (40 ml) was stirred under nitrogen for 48 h. The solvent was removed in vacuo and the residue was dissolved in diethylene glycol (30 ml) and heated at 200° for 2 h. The solution was allowed to cool, poured into water (200 ml) and extracted with dichloromethane (3×100 ml). The combined, dried organic extracts were evaporated to give an oil (ca. 2.5 g) which was purified by short path column chromatography on silica gel (Merck 7729) eluting with System A (400:10:1) to give the title compound (330 mg) as a solid, m.p. 265°-267°.

1. customThe solvent was removed in vacuo
2. dissolutionthe residue was dissolved in diethylene glycol (30 ml)
3. temperatureheated at 200° for 2 h
4. temperatureto cool
5. additionpoured into water (200 ml)
6. extractionextracted with dichloromethane (3×100 ml)
7. customdried organic extracts were evaporated