HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 47015344, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| Reactant | 2,5-Difluorobenzoyl chloride | HCID 588082 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 47015344 | HCID 47015344 | 74.8% |
Reaction Steps
To a mixture of 2,5-difluorobenzoyl chloride (1.77 g, 10 mmol) and O-methylhydroxylamine hydrochloride (830 mg, 10 mmol) in methylene chloride (25 mL) at 0° C. was added dropwise triethylamine (2.8 mL, 20 mmol) and the mixture was stirred at room temperature for 8 h. The mixture was then washed with water, brine, dried with MgSO4 and concentrated under reduced pressure. The residue was chromatographed (hexane-EtOAc 2:1) to afford 1.4 g of the title compound. 1H NMR (300 MHz-DMSO-d6) δ 3.70 (s, 3H), 7.42 (m, 3H), 11.64 (s, 1H); MS (DCI/NH3) m/z 188 (M+H)+, 205 (M+NH4)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07875640B2 |
| Source dataset | uspto-grants-2011_01 |
| ORD ID | ord-ea44832183364fda90a669263e92aa73 |
| Source note | uspto-grants-2011_01 |