HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 68600944, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Methoxy-N-methylaniline | HCID 2759579 | — |
| Reactant | HCID 86642580 | HCID 86642580 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68600944 | HCID 68600944 | 77.8% |
Reaction Steps
2-Methoxy-N-methylaniline (7.4 g, 53.8 mmol) and triethylamine (10.9 g, 107.7 mmol) were added to 5-bromo-4-chloro-2-fluoro-benzoyl chloride (Step 21D, 11.7 g, 43.1 mmol) in DCM (200 mL) at 0° C. The mixture was then allowed to warm to rt and concentrated. The mixture was partitioned in water and ethyl acetate. The organic layer was separated, washed with NaHSO4 solution, water and brine, and was dried. After filtration and concentration, the residue was purified via silica gel flash column chromatography eluting with ethyl acetate in hexane (50%) to give 5-bromo-4-chloro-2-fluoro-N-(2-methoxy-phenyl)-N-methyl-benzamide (12.5 g). MS: [M+H]+374.0/372.0; tR=2.70 min (method 1)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481738B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-9b4f459f23754e318f6ac2b85e20347e |
| Source note | uspto-grants-2013_07 |