反应详情

To 240 ml of methanol containing 8.0 g of potassium hydroxide, 8.12 g (17.2 mmol) of 4-chloro-6-[(2-ethyl-5,7-dimethyl-3H-imidazo[4,5-b]pyridin-3-yl)methyl]-2-(nitrophenyl)quinoline obtained in Example 4 and 0.80 g of a 5% palladium-carbon catalyst were added and the thus-prepared mixture was stirred under a hydrogen atmosphere for 17 hours. After adding 120 ml of chloroform thereto, the thus-prepared mixture was filtered through celite. To the resulting filtrate, 120 ml of water was added, and the thus-prepared mixture was then separated out. The resulting organic layer was washed with 120 ml of water. Then, 60 ml of water was added to the organic layer, and a 130 ml portion thereof was distilled off by heating under atmospheric pressure. After allowing to stand at 0° C., the crystals precipitated were collected by filtration, and the resulting filtration residue was further recrystallized from a mixture of chloroform with methanol to obtain 3.30 g of 2-{6-[(2-ethyl-5,7-dimethyl-3H-imidazo[4,5-b]pyridin-3-yl)methyl]quinolin-2-yl}aniline.

1. filtrationthe thus-prepared mixture was filtered through celite
2. additionTo the resulting filtrate, 120 ml of water was added
3. customthe thus-prepared mixture was then separated out
4. washThe resulting organic layer was washed with 120 ml of water
5. additionThen, 60 ml of water was added to the organic layer
6. distillationa 130 ml portion thereof was distilled off
7. temperatureby heating under atmospheric pressure
8. customto stand at 0° C.
9. customthe crystals precipitated
10. filtrationwere collected by filtration
11. filtrationthe resulting filtration residue
12. customwas further recrystallized from a mixture of chloroform with methanol