反应详情

2,8-Dimethyl-1-oxa-8-azaspiro[4.5]decan-3-one (1.0 g, 5.5 mmol) and semicarbazide hydrochloride (1 g) were dissolved in abs. EtOH (50 ml). The reaction was stirred at room temperature overnight. The reaction was concentrated in vacuo and the residue was dissolved in chloroform and washed with saturated Na2CO3. The chloroform layer was dried and concentrated to give the crude product which was purified by chromatography on silica gel and elution with ammoniated 2-10% MeOH/CHC3. The solid obtained (1.4 g) was converted to the maleate salt in hot ethyl acetate. The resulting solid was digested with hot ethyl acetate and dried to give the title product, mp 204°-206° C.

1. concentrationThe reaction was concentrated in vacuo
2. dissolutionthe residue was dissolved in chloroform
3. washwashed with saturated Na2CO3
4. dry with materialThe chloroform layer was dried
5. concentrationconcentrated
6. customto give the crude product which
7. customwas purified by chromatography on silica gel and elution with ammoniated 2-10% MeOH/CHC3
8. customThe solid obtained (1.4 g)
9. customdried