HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → HCID 86597701, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 86597700 | HCID 86597700 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 86597701 | HCID 86597701 | 78% |
Reaction Steps
To a solution of 150 mg (0.227 mmol) (R)-2-(3,5-bis-trifluoromethyl-phenyl)-N-[4-(4-fluoro-2-methyl-phenyl)-6-(3-methanesulfonylamino-pyrrolidin-1-yl)-pyridin-3-yl]-N-methyl-isobutyramide in 1 ml dimethylformamide were added 15 mg (0.34 mmol) sodium hydride (55% dispersion in mineral oil) at room temperature. After stirring at room temperature for 30 min 39 mg (27 mmol) iodomethane were added. The reaction mixture was stirred at room temperature for 18 h, followed by dilution with 10 ml ethyl acetate and washing with 10 ml saturated sodium carbonate solution. The combined organic layers were dried over sodium sulfate, concentrated in vacuo and purified by flash chromatography to give 120 mg (78%) of the title compound as a white foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07939533B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-7455f45da44445d6aed437c5294bc450 |
| Source note | uspto-grants-2011_05 |