HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 14574473, compound → HCID 178497326, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 14574473 | HCID 14574473 | — |
| Catalyst | Platinum | HCID 23939 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 178497326 | HCID 178497326 | 60.1% |
Reaction Steps
A mixture of dimethyl 4-acetamido-3-nitrophthalate (142.1 g, 0.480 mol) in methanol with 5% platinum on carbon catalyst is hydrogenated on a Parr hydrogenator at room temperature. The reaction mixtures is filtered through diatomaceous earth and concentrated in vacuo to afford a solid residue. This solid is dispersed in glacial acetic acid and toluene, and heated with stirring at reflux temperatures for 4 hours with azeotropic removal of water. The resultant hot reaction mixture is slowly added to a saturated sodium bicarbonate solution with vigorous stirring, filtered and the filter cake dried to give the title product as a white solid (71.6 g, 60.1%), mp 97°-103° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05523279 |
| Source dataset | uspto-grants-1996_06 |
| ORD ID | ord-ad91672629d34457b9f18f3982367648 |
| Source note | uspto-grants-1996_06 |