HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 71254826, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | 3-Chloro-2-fluorobenzaldehyde | HCID 736335 | — |
| Reactant | HCID 56776464 | HCID 56776464 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 71254826 | HCID 71254826 | 92% |
Reaction Steps
(E)-3-Chloro-2-fluorobenzaldehyde oxime: To the solution of 3-chloro-2-fluorobenzaldehyde (1.3 g, 8.20 mmol) and hydroxylamine hydrochloride (0.695 g, 10.00 mmol) in EtOH (6.83 mL)/water (6.83 mL) was added 1 N NaOH (10.00 mL, 10.00 mmol). The reaction was stirred at rt for 4 h, then it was acidified to pH 6 with 1 N HCl which gave a white suspension. The reaction mixture was filtered, and the solid was rinsed with water, and air-dried to afford the desired product (1.31 g, 92%) as a white solid. MS(ESI) m/z: 174.0 (M+H)+. 1H NMR (500 MHz, CDCl3) δ 8.36 (s, 1H), 7.74 (s, 1H), 7.66 (ddd, J=7.8, 6.3, 1.7 Hz, 1H), 7.42 (ddd, J=8.0, 7.2, 1.7 Hz, 1H), 7.13-7.07 (m, 1H) ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09221818B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-238e61cde72249ca8e5c00b9133e95ca |
| Source note | uspto-grants-2015_12 |