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Dimethylformamide → 1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 4-(4-Fluorobenzoyl)-1-(2-hydroxyethyl)piperidine | HCID 14892165 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(2-Chloroethyl)-4-(4-fluorobenzoyl)piperidine hydrochloride | HCID 67575338 | 96.3% |
反応手順
In an atmosphere of dry air, 4-(4-fluorobenzoyl)-1-(2-hydroxyethyl)piperidine (1.96 g, 7.8 mmol) was dissolved in methylene chloride (10 ml) to which, with cooling in an ice bath, were subsequently added dropwise DMF (0.1 ml) and thionyl chloride (2.5 ml, 34.2 mmol). After 7 hours of stirring at room temperature, the solvent was removed by evaporation, and the resulting residue was subjected to azeotropic distillation using benzene (15 ml×2). Thereafter, the thus obtained residue was washed with an ether-methylene chloride (4:1) mixture solution (30 ml) to obtain 2.3 g (96.3%) of the title compound in the form of light beige powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05728835 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-761b0c03342a44cd91f901367699772b |
| 出典メモ | uspto-grants-1998_03 |