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Tetrahydrofuran → 4-(2-Methylpropyl)-3-(trifluoromethyl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 4-Bromo-3-(trifluoromethyl)benzonitrile | HCID 10800647 | — |
| 反応物 | HCID 178448254 | HCID 178448254 | — |
| 生成物 | 4-(2-Methylpropyl)-3-(trifluoromethyl)benzamide | HCID 57057862 | — |
反応手順
To a solution of 4-bromo-3-trifluoromethylbenzonitrile (1.25 g, 5.0 mmol) and isobutylzinc bromide (25 mmol) in THF (50 mL, 25 mmol) under argon was added 1,1′-bis(diphenylphosphino)ferrocenedichloro palladium(II) dichloromethane complex (612 mg, 0.75 mmol) and the reaction heated at reflux for 5 h. The mixture was concentrated in vacuo and the residue partitioned between ethyl acetate (80 mL) and water (80 mL). A solid formed and was filtered off and discarded. The organic layer was washed with water (80 mL) before it was dried (phase separator) and concentrated in vacuo to give the crude title compound as a black oil. This was used directly in the next step (1.35 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08101775B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-dc994e21b9f242e2a9dc24413ccd496b |
| 出典メモ | uspto-grants-2012_01 |