反应详情

温度

50 °C

A 250-ml heater-equipped autoclave pressure bottle was charged with a solution of 20 (16.0 g) in aniline (40 ml), containing catalyst platinum oxide (0.075 g). The mixture was agitated vigorously at 50° C. and 60 psi of hydrogen until no further pressure drop was observed (3-4 h). The reaction mixture was filtered and concentrated under reduced pressure to 10 ml and poured slowly into hexane. The hexane was decanted off. The light brown paste was then extracted with hot hexane until the maceration was difficult. The thick paste was cooled in ice to give a light-yellow solid, which recrystallized from o-dichlorobenzene to give a white solid. The solid was further boiled with n-hexane, filtered, and dried to yield 21 (10.0 g). DTA examination of this solid showed a melting point range from 115°-145° C.

1. customA 250-ml heater-equipped autoclave pressure bottle
2. custom(3-4 h)
3. filtrationThe reaction mixture was filtered
4. concentrationconcentrated under reduced pressure to 10 ml
5. additionpoured slowly into hexane
6. customThe hexane was decanted off
7. extractionThe light brown paste was then extracted with hot hexane until the maceration
8. temperatureThe thick paste was cooled in ice
9. customto give a light-yellow solid, which
10. customrecrystallized from o-dichlorobenzene
11. customto give a white solid
12. filtrationfiltered
13. customdried