HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4-Amino-2-(methoxycarbonyl)-3-methyl-5-nitrobenzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 4-Amino-3-methyl-5-nitro-phthalic acid dimethyl ester | HCID 59761781 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-Amino-2-(methoxycarbonyl)-3-methyl-5-nitrobenzoic acid | HCID 59761680 | 76.1% |
Reaction Steps
To a solution of 4-Amino-3-methyl-5-nitro-phthalic acid dimethyl ester (1.8 g, 6.72 mmol) in THF (10 mL) and water (20 mL) was added 5 N NaOH (4.0 mL) and the resulting mixture was stirred at room temperature for 24 h. The reaction mixture was acidified with conc. HCl (pH=2.0) and extracted with EtOAc (2×100 mL). The combined organic layer was dried over Na2SO4, filtered and concentrated in vacuo to afford the 4-Amino-3-methyl-5-nitro-phthalic acid 2-methyl ester (1.3 g, 76%) as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09290503B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-7a84e096ed254391bbd0e7f8b06e9bc1 |
| Source note | uspto-grants-2016_03 |