反应详情

Azetidine (0.36 g, 0.5 mmol) was added to N-{1-[N-(benzyloxycarbonyl)-sulfamoyl]pyridin-4(1H)-ylidene}-N-methylmethanaminium chloride (Preparation 21, 2.0 g, 0.5 mmol) in DCM (10 mL). The reaction mixture was stirred overnight at room temperature. The mixture was concentrated in vacuo and the residue partitioned between ethyl acetate (50 mL) and water (50 mL). The organic layer was discarded and the aqueous layer was acidified with 1M HCl. The aqueous layer was extracted with ethylacetate (2×50 mL), dried over magnesium sulfate and concentrated to afford the title compound (1.49 g, 100%).

1. concentrationThe mixture was concentrated in vacuo
2. customthe residue partitioned between ethyl acetate (50 mL) and water (50 mL)
3. extractionThe aqueous layer was extracted with ethylacetate (2×50 mL)
4. dry with materialdried over magnesium sulfate
5. concentrationconcentrated