HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 2,4-Difluoro-benzaldehyde oxime
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 2,4-Difluorobenzaldehyde | HCID 73770 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | 2,4-Difluoro-benzaldehyde oxime | HCID 53395027 | 94.6% |
Reaction Steps
(Scheme 1, Compound C) To a mixture of 2,4-difluorobenzaldehyde (0.80 g, 5.6 mmol) and hydroxyamine HCl salt (0.43 g, 6.2 mmol) in EtOH (5 mL) was added K2CO3 (0.85 g, 6.2 mmol). The resultant mixture was stirred at rt for 24 hours. The mixture was diluted with MeOH (20 mL). The precipitates were filter off and washed with MeOH. The product from filtrate was purified by recrystalization (EtOAc/Hexanes). This compound was obtained as a white solid (0.84 g, 5.3 mmol, 94% yield). 1H NMR (DMSO-d6) δ 12.98 (br. s, 1H), 8.17 (s, 1H), 7.79 (m, 1H), 7.32 (m, 1H), 7.11 (m, 1H); Analytical HPLC 1.03 min. (95%); Mass Spec.: 158.06 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06949574B2 |
| Source dataset | uspto-grants-2005_09 |
| ORD ID | ord-069ed5cc32b84dba804f8537909d11f8 |
| Source note | uspto-grants-2005_09 |