HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → N-(3(2-((dimethylamino)methyl)-1H-imidazol-1-yl)-5-(trifluoromethyl)phenyl)-3-iodo-4-methylbenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 3-Iodo-4-methylbenzoyl chloride | HCID 17752157 | — |
| Reactant | 3-(2-((Dimethylamino)methyl)-1H-imidazol-1-yl)-5-(trifluoromethyl)aniline | HCID 46838610 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | N-(3(2-((dimethylamino)methyl)-1H-imidazol-1-yl)-5-(trifluoromethyl)phenyl)-3-iodo-4-methylbenzamide | HCID 46838614 | — |
Reaction Steps
3-Iodo-4-methylbenzoyl chloride (2.2 g, 7.88 mmol), dissolved in anhydrous THF (13 mL), was added dropwise to a solution of 3-(2-((dimethylamino)methyl)-1H-imidazol-1-yl)-5-(trifluoromethyl)aniline (1.5 g, 5.5 mmol), DIPEA (2.1 mL, 11.8 mmol) in THF (30 mL) at ˜5° C. The resultant solution was stirred at ambient temperature overnight. The solvent was removed in vacuo and the crude residue was redissolved in CH2Cl2 and washed with 1N NaOH. The organic layer was then washed with water, and brine then dried over NaSO4 before being concentrated in vacuo. The brown colored residue was then triturated in a mixture of hexanes/DCM to precipitate 1.4 g of the desired product as an off-white powder: 529 m/z (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09278971B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-ad2bd85b00d247c0940732a37185cccd |
| Source note | uspto-grants-2016_03 |