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Sulfuric Acid → N-(1-benzyl-3-methylpyrrolidin-3-yl)acetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 1-Benzyl-3-methylpyrrolidin-3-OL | HCID 18629648 | — |
| 生成物 | N-(1-benzyl-3-methylpyrrolidin-3-yl)acetamide | HCID 13787481 | 50% |
反応手順
To a solution of 1-benzyl-3-methylpyrrolidin-3-ol (1.0 g, 5.2 mmol) in acetonitrile (10 mL) at 0° C., was added concentrated sulfuric acid (10 mL) slowly. After being stirred for 16 hours at room temperature, the reaction mixture was poured into ice-water. After the reaction mixture was adjusted to pH 7 with a saturated aqueous solution of potassium carbonate, the resulting mixture was exacted with dichloromethane (200 mL×3). The combined organic layers were dried over sodium sulfate, and concentrated in vauo. The residue was purified by preparative HPLC to afford 600 mg of the product (yield was 50%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08871756B2 |
| 出典データセット | uspto-grants-2014_10 |
| ORD ID | ord-8ccc0ee2e02f400c8e620e39af55cf5b |
| 出典メモ | uspto-grants-2014_10 |