反应详情

2-(5-Phenoxymethyl-pyridin-2-ylmethyl)-isoindol-1,3-dione described in Preparation Example 188 (383 mg, 1.11 mmol) was dissolved in ethanol (3 mL) and tetrahydrofuran (3 mL). Hydrazine monohydrate (538 μL, 11.1 mmol) was added to this solution at room temperature, and the solution was stirred under reflux for 1 hour. The reaction solution was partitioned in water and ethyl acetate. The organic layer was separated, washed with brine, and then, dried over anhydrous magnesium sulfate. The organic layer was filtered, then, the solvent was evaporated in vacuo, the residue was purified by NH silica gel column chromatography (ethyl acetate/methanol=10/1), and the title compound (122 mg, 51%) was obtained as a colorless oil.

1. temperatureunder reflux for 1 hour
2. customThe reaction solution was partitioned in water
3. customThe organic layer was separated
4. washwashed with brine
5. dry with materialdried over anhydrous magnesium sulfate
6. filtrationThe organic layer was filtered
7. customthe solvent was evaporated in vacuo
8. customthe residue was purified by NH silica gel column chromatography (ethyl acetate/methanol=10/1)