反应详情

1 l of methanol was mixed with 77 g of the crude N-{1-(6-chloropyridin-2-yl)-2-(pyridin-2-yl)ethyl}-phthalimide prepared in the Preparative Example 23 and 16.5 g of hydrazine monohydrate. The obtained mixture was heated under reflux for 2 hours to conduct a reaction. After the reaction mixture was allowed to stand at room temperature, the precipitated crystals were filtered out and the filtrate was concentrated. Water and ethyl acetate were added to the concentrate to conduct extraction. The organic phase was washed with a saturated aqueous solution of common salt, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by silica gel chromatography (with a methanol/dichloromethane (5:95 mixture) to give 22.38 g of the title compound.

1. temperatureThe obtained mixture was heated
2. temperatureunder reflux for 2 hours
3. customa reaction
4. customto stand at room temperature
5. filtrationthe precipitated crystals were filtered out
6. concentrationthe filtrate was concentrated
7. additionWater and ethyl acetate were added to the
8. concentrationconcentrate
9. extractionextraction
10. washThe organic phase was washed with a saturated aqueous solution of common salt
11. dry with materialdried over anhydrous sodium sulfate
12. concentrationconcentrated
13. customThe residue was purified by silica gel chromatography (with a methanol/dichloromethane (5:95 mixture)