HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 3-Fluoro-2-(2H-1,2,3-triazol-2-yl)benzoic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Methanol | HCID 887 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 3-Fluoro-2-(2H-1,2,3-triazol-2-yl)benzonitrile | HCID 67086447 | — |
| Product | 3-Fluoro-2-(2H-1,2,3-triazol-2-yl)benzoic acid | HCID 67086549 | 18% |
Reaction Steps
To 3-fluoro-2-(2H-1,2,3-triazol-2-yl)benzonitrile (1.5 g, 8.0 mmol) in MeOH (30 mL) was added 2M aq. NaOH (10 mL). The reaction was heated at reflux for 15 h, then cooled to rt, acidified with 1N aq. HCl to pH=1 and extracted with DCM (2×). The combined organics were washed with brine and dried (Na2SO4). Purification via Agilent (Reverse-Phase HPLC, basic conditions) gave the title compound (290 mg, 18%). 1H NMR (CDCl3): 7.90 (s, 2H), 7.89-7.85 (m, 1H), 7.63-7.56 (m, 1H), 7.50-7.44 (m, 1H) and 3-methoxy-2-(2H-1,2,3-triazol-2-yl)benzoic acid (Intermediate 53, 140 mg, 8%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653263B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-4292a33d35d748f093044e20cc4de070 |
| Source note | uspto-grants-2014_02 |