反应详情

3,5-dinitro-p-toluic acid (10.0 gm.) is dissolved in methanol (300 ml.) and 5% palladium on charcoal (1.0 gm.) added. Reduction is carried out in a Parr apparatus for one hour at 40 psi of hydrogen. The product precipitates and the reaction mixture warmed until solution is complete. The catalyst is removed by filtration, washed with a few cc of methanol and the filtrate cooled to 0°. The product precipitates in fine needles and is collected by filtration, washed with a few ml. of methanol and dried (5.95 gm., 81% yield, m.p. 218°-200° dec.). The thin layer chromatogram (Silica gel, 5% methanol in chloroform) shows the material to be homogeneous.

1. customThe product precipitates
2. temperaturethe reaction mixture warmed until solution
3. customThe catalyst is removed by filtration
4. washwashed with a few cc of methanol
5. temperaturethe filtrate cooled to 0°
6. customThe product precipitates in fine needles
7. filtrationis collected by filtration
8. washwashed with a few ml
9. dry with materialof methanol and dried (5.95 gm., 81% yield, m.p. 218°-200° dec.)