反应详情

Hydrazine monohydrate (0.11 mL, 2.35 mmol) was added to a solution of tert-butyl {3-[(dimethylamino)methylene]-4-oxocyclohexyl}carbamate obtained in Example (242a) (526 mg, 1.96 mmol) in methanol (10 mL), and the mixture was heated under reflux for 18 hours. The reaction solution was concentrated. The resulting residue was azeotropically distilled with toluene and then purified by silica gel column chromatography (elution solvent: dichloromethane/methanol 20/1) to obtain 257 mg of the title compound as an amorphous compound (55%).

1. temperaturethe mixture was heated
2. temperatureunder reflux for 18 hours
3. concentrationThe reaction solution was concentrated
4. distillationThe resulting residue was azeotropically distilled with toluene
5. custompurified by silica gel column chromatography (elution solvent: dichloromethane/methanol 20/1)