n-methyl-3-nitroaniline → N1-Methylbenzene-1,3-diamine

Temperature

70 °C

8 g of the precipitate was dissolved in 20 mL of 95% ethanol, 1 g of a catalyst having 5 wt. % Pd on a carbon support was added and hydrogenation of the N-methyl-3-nitroaniline was carried out at 50 psig (337 kPa gage) for about 10 minutes, during which time the temperature increased to about 70° C. The hydrogenated mixture was cooled to room temperature, filtered to recover the solids, which were then washed with methanol and the liquid filtrates combined. Finally, the liquids were concentrated under vacuum and distilled through a short path Kugelrohr oven at about 140° C. and 3 torr to produce a 96% yield of N-methyl m-phenylenediamine.

1. additionwas added
2. temperatureThe hydrogenated mixture was cooled to room temperature
3. filtrationfiltered
4. customto recover the solids, which
5. washwere then washed with methanol
6. concentrationFinally, the liquids were concentrated under vacuum
7. distillationdistilled through a short path Kugelrohr oven at about 140° C.

ORD record

ord-c1390334349e4e319cc0af1081c1e4f5

Source dataset

uspto-grants-1993_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05234598