反应详情

A mixture of 2-[3-(4-trifluoromethylphenyl)-2-propenyl]phthalimide (4.57 g, 13.79 mmol) prepared in Reference Example 102 and hydrazine hydrate (897 mg, 17.93 mmol) in ethanol (80 ml) was heated under reflux for 3 hours. The reaction mixture was allowed to return to room temperature and filtered, and the filtrate was concentrated under reduced pressure. To the residue, ethyl acetate was added, and the resulting mixture was washed with 1 N sodium hydroxide aqueous solution and brine, and dried over magnesium sulfate. After filtration, the filtrate was concentrated under reduced pressure to afford 3-(4-trifluoromethylphenyl)-2-propenylamine (2.78 g, quantitative) as a pale brown crystalline powder.

1. temperaturewas heated
2. temperatureunder reflux for 3 hours
3. customto return to room temperature
4. filtrationfiltered
5. concentrationthe filtrate was concentrated under reduced pressure
6. additionTo the residue, ethyl acetate was added
7. washthe resulting mixture was washed with 1 N sodium hydroxide aqueous solution and brine
8. dry with materialdried over magnesium sulfate
9. filtrationAfter filtration
10. concentrationthe filtrate was concentrated under reduced pressure