HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 2177297-18-4
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | N-(1-Methylethyl)ethanamide | HCID 136874 | — |
| Reactant | 4-Bromo-2,6-difluoroaniline | HCID 610191 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 2177297-18-4 | HCID 67426737 | 100% |
Reaction Steps
Add TEA (10.05 mL) to a mixture of 4-bromo-2,6-difluoro-phenylamine (10.0 g), N-isopropyl acetamide (9.73 g), phosphoryl chloride (6.70 mL) in toluene (150 mL). Heat the mixture to reflux for 3 h. Cool the mixture and remove the solvent under vacuum. Dissolve the crude in DCM, wash with an aqueous saturated solution of sodium bicarbonate several times to remove all traces of acid. Dry over sodium sulfate and remove the solvent under vacuum to afford 14 g of the title compound. MS (ES+): m/z=292 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07855211B2 |
| Source dataset | uspto-grants-2010_12 |
| ORD ID | ord-a60ff680a524485e82e4d18e7965283b |
| Source note | uspto-grants-2010_12 |