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Benzyl Bromide → 2-benzyloxy-N-[3,5-bis(trifluoromethyl)phenyl]-5-chloro-benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Imd-0354 | HCID 5081913 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-benzyloxy-N-[3,5-bis(trifluoromethyl)phenyl]-5-chloro-benzamide | HCID 71508592 | 93% |
反応手順
N-(3,5-bis(trifluoromethyl)phenyl)-5-chloro-2-hydroxybenzamide (191.8 mg) obtained in step 1 was dissolved in dimethylformamide (DMF, 1.5 ml), to which benzylbromide (0.07 ., 0.55 mmol) and potassium carbonate (K2CO3, 82.9 mg, 0.6 mmol) were added. The reaction mixture was stirred at room temperature for 4 hours. Dimethylformamide was distillated under reduced pressure, followed by extraction with ethylacetate (EtOAc). The extracted organic layer was dried over MgSO4, filtered and concentrated. The concentrated reactant was separated by column chromatography (developing solvent: hexane/ethylacetate=15/1) to give 220 mg of the target compound (yield: 93%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09266872B2 |
| 出典データセット | uspto-grants-2016_02 |
| ORD ID | ord-40de91f884a44fcda94fb99ecc2b1564 |
| 出典メモ | uspto-grants-2016_02 |