反应详情

Acetic acid (40 ml) and pyridine-borane (4.3 ml) were added to 2-{[1-(4-methoxy-3-methylphenyl)-methylidene]amino}isoindole-1,3-dione (2.50 g) prepared in the Step 15-1-1, and the mixture was stirred under a room temperature for 0.5 hours. The mixture was concentrated under a reduced pressure, and under an ice cooling 10% hydrochloric acid (10 ml) was added to the resulting residue. Sodium hydroxide (1.1 g) was added thereto, and the resulting mixture was subjected to extraction with ethyl acetate. The organic layer was washed with a saturated saline solution, and then dried over sodium sulfate and concentrated under a reduced pressure. To the resulting residue, ethanol (10 ml) was added, and the mixture was stirred at a room temperature. The precipitate was separated by filtration, washed with ethanol, and concentrated under a reduced pressure to give the title compound (1.71 g, 68%).

1. customprepared in the Step 15-1-1
2. concentrationThe mixture was concentrated under a reduced pressure
3. additionunder an ice cooling 10% hydrochloric acid (10 ml) was added to the resulting residue
4. additionSodium hydroxide (1.1 g) was added
5. extractionthe resulting mixture was subjected to extraction with ethyl acetate
6. washThe organic layer was washed with a saturated saline solution
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated under a reduced pressure
9. additionTo the resulting residue, ethanol (10 ml) was added
10. stirringthe mixture was stirred at a room temperature
11. customThe precipitate was separated by filtration
12. washwashed with ethanol
13. concentrationconcentrated under a reduced pressure