関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Chlorodiphenylmethane | HCID 7035 | — |
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(Diphenylmethyl)pyrrolidine | HCID 245012 | 61.4% |
反応手順
Chlorodiphenylmethane (0.50 g, 2.47 mmol) (Wako Pure Chemical Industries, Ltd.), pyrrolidine (0.53 g, 7.45 mmol) (Tokyo Chemical Industry Co., Ltd.), and potassium iodide (0.10 g, 0.60 mmol) (Wako Pure Chemical Industries, Ltd.) were added to acetonitrile (20 mL) (Wako Pure Chemical Industries, Ltd.), and the mixture was refluxed for 2 hours. The mixture was allowed to cool to room temperature. After that, a saturated aqueous solution of sodium hydrogen carbonate (Wako Pure Chemical Industries, Ltd.) was added to the reaction solution, and mixture was extracted with ethyl acetate (Wako Pure Chemical Industries, Ltd.). The organic layer was dried with anhydrous sodium sulfate (Wako Pure Chemical Industries, Ltd.), and the solvent was distilled off under reduced pressure. The residue was subjected to silica gel column chromatography (chloroform (Wako Pure Chemical Industries, Ltd.):methanol (Wako Pure Chemical Industries, Ltd.)=99:1 as an eluent), to thereby obtain the title compound (0.36 g, 61% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846012B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-538c707c4b594608ab700e0bee2c52fc |
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| 出典メモ | uspto-grants-2014_09 |
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