HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-Methyl-4-nitrobenzoic acid → 4-Amino-3-methylbenzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-Methyl-4-nitrobenzoic acid | HCID 18370 | — |
| Catalyst | Nickel | HCID 935 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 4-Amino-3-methylbenzoic acid | HCID 75598 | — |
Reaction Steps
To a solution of 3-methyl-4-nitro-benzoic acid (100 g, 0.55 mol) in DMF (500 mL), suspension of activated Raney Ni (50 g) in DMF (50 mL) was added and was subjected to hydrogenation (200 psi pressure and 25° C.) for 6 h. The reaction mixture was filtered through celite bed and was concentrated to one third of the total volume. The reaction mixture was poured into water (1300 mL) with stirring. The solid was filtered, washed with water and dried to obtain the title compound. Yield: 70 g (84%); 1H NMR (DMSO-d6, 300 MHz): δ 2.03 (s, 3H, CH3), 5.60 (s, 2H, NH2), 6.56 (d, 1H, Ar), 7.46 (d, 1H, Ar), 7.49 (s, 1H, Ar); MS: m/e (ES−) 150 (M−1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08163730B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-18ee0747478844d68af0c50b8a967685 |
| Source note | uspto-grants-2012_04 |