化工社化工社 化学情報印刷レポート · 研究参考用
Sodium hydride → (S)-[(3,4-Difluorophenoxy)methyl]-oxirane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 3,4-Difluorophenol | HCID 75927 | — |
| 反応物 | Oxiranemethanol, 4-methylbenzenesulfonate, (S)- | HCID 153296 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (S)-[(3,4-Difluorophenoxy)methyl]-oxirane | HCID 53482062 | 51.1% |
反応手順
To a stirred and cooled (ice-bath) mixture of 13.0 g of 3,4-difluorophenol and 200 ml of N,N-dimethylformamide, there were added 4.8 g of a dispersion of sodium hydride in mineral oil (50%) and, after stirring for 1 hour, a solution of 22.8 g of (S)-(oxiranylmethyl) 4-methylbenzenesulfonate (ester) in some N,N-dimethylformamide. Stirring at room temperature was continued overnight. The reaction mixture was poured into ice-water and the product was extracted with methylbenzene. The extract was washed with NaCl (dil.) and water and was then dried, filtered and evaporated. The residue was distilled (13.3 Pa, 55° C.), yielding 9.5 g (51.0%) of (S)-[(3,4-difluorophenoxy)methyl]oxirane (interm. 1 ).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05530011 |
| 出典データセット | uspto-grants-1996_06 |
| ORD ID | ord-f4c0909046dc4f19bd7e05b9176bdb8d |
| 出典メモ | uspto-grants-1996_06 |