HuagongsheHuagongshe Chemistry Print Report · For research reference only
Formic Acid → HCID 5328451, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Formic Acid | HCID 284 | — |
| Reactant | HCID 68667054 | HCID 68667054 | — |
| Solvent | Trimethyl orthoformate | HCID 9005 | — |
| Product | HCID 5328451 | HCID 5328451 | 90% |
Reaction Steps
A stirred solution of give 4-(2-aminophenylamino)benzoic acid methyl ester (13 g, 0.054 mol) in trimethyl orthoformate was treated with formic acid (13 mL), heated at reflux temperature for 1 h, cooled to room temperature and concentrated in vacuo. The residual oil was purified by column chromatography (silica, CHCl3/MeOH 1%) to give the title compound in 90% yield, 1H NMR (400 MHz, CDCl3): 8.26-8.28 (m, 3H), 8.17 (s, 1H), 7.90 (bs, 1H), 7.63 (d, J=8.8 Hz, 2H), 7.59 (m, 1H), 7.40 (m, 1H), 7.26 (s, 1H). 3.9 (s, 3H). LCMS (ESI+) 253 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07803825B2 |
| Source dataset | uspto-grants-2010_09 |
| ORD ID | ord-2b746ad33aa54a8783a950a99a4b35e3 |
| Source note | uspto-grants-2010_09 |