HuagongsheHuagongshe Chemistry Print Report · For research reference only
5-Nitrosalicylic acid → HCID 9882573, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 5-Nitrosalicylic acid | HCID 7318 | — |
| Reactant | 2,4-Difluoroaniline | HCID 9709 | — |
| Reactant | Phosphorus trichloride | HCID 24387 | — |
| Solvent | Chlorobenzene | HCID 7964 | — |
| Product | HCID 9882573 | HCID 9882573 | 35% |
Reaction Steps
A solution of 5-nitrosalicylic acid (1.4 g, 7.7 mmol) and 2,4-difluoroaniline (0.8 mL, 7.7 mmol) in chlorobenzene (40 mL) was treated with PCl3 (0.338 mL, 3.8 mmol). The solution was heated at reflux under an argon atmosphere. After 2 h. the solution was filtered hot and the filtrate was left standing at RT. After 18 h the solution was filtered and the solid was recrystallized from MeOH to give the title compound (0.733 g, 35% yield): 1H NMR (400 MHz, DMSO-d6) δ 2.5-2.6 (s, 3H), 7.1-8.9 (m, 6H), 10.6-10.7 (s, 1H)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06492425B1 |
| Source dataset | uspto-grants-2002_12 |
| ORD ID | ord-8bed730f5c464ab0a0c89d54deec7e6f |
| Source note | uspto-grants-2002_12 |