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Ammonium Chloride → N-(3-cyclohexylphenyl)-4-hydroxy-3-methoxyphenylacetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 4-hydroxy-N-(3-iodophenyl)-3-methoxyphenylacetamide | HCID 12096660 | — |
| 反応物 | HCID 178418970 | HCID 178418970 | — |
| 触媒 | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-(3-cyclohexylphenyl)-4-hydroxy-3-methoxyphenylacetamide | HCID 9881043 | — |
反応手順
Intermediate 1 (850 mg) and tetrakis(triphenylphosphine)-palladium (0) (250 mg) are dissolved in tetrahydrofuran (16 ml), and thereto is added a 0.5 M tetrahydrofuran solution (20 ml) of cyclohexylzinc bromide under argon atmosphere at room temperature, and the mixture is stirred for 18 hours. A saturated aqueous ammonium chloride solution is added to the reaction solution, and the mixture is extracted with ethyl acetate. The organic layer is dried over sodium sulfate, and the solvent is evaporated under reduced pressure. The residue is purified by silica gel column chromatography (eluent: gradient from 0% to 100% hexane/ethyl acetate) to give the desired compound (120 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084176B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-b59d64d91f264abeae1d4d6a9e60e2b0 |
| 出典メモ | uspto-grants-2006_08 |