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Benzyl Bromide → Benzyl 3-oxo-3-{[3-(trifluoromethyl)phenyl]amino}propanoate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzyl Bromide | HCID 7498 | — |
| 反応物 | Lithium 3-oxo-3-{[3-(trifluoromethyl)phenyl]amino}propanoate | HCID 23693664 | — |
| 触媒 | Trioctylmethylammonium chloride | HCID 21218 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Benzyl 3-oxo-3-{[3-(trifluoromethyl)phenyl]amino}propanoate | HCID 59666221 | — |
反応手順
To a stirred solution of lithium 3-oxo-3-{[3-(trifluoromethyl)phenyl]amino}propanoate (2.0 g, 7.9 mmol) (Example 2A) in water (15 ml) is added a solution of Aliquat 336® (3.1 g) and benzyl bromide (1.35 g, 7.5 mmol) in dichloromethane (15 ml). The reaction mixture is stirred for two days at room temperature, then extracted with dichloromethane (500 ml). The organic phase is dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo. The residue is purified by flash chromatography over silica gel 60 with cyclohexane/ethyl acetate mixtures as eluent.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08097629B2 |
| 出典データセット | uspto-grants-2012_01 |
| ORD ID | ord-668855b86b7c461f877532ce50aa3ef7 |
| 出典メモ | uspto-grants-2012_01 |