化工社化工社 化学情報印刷レポート · 研究参考用
2,4-Dichlorophenol → 2,4-Dichloro-1-methylsulfanylmethoxy-benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,4-Dichlorophenol | HCID 8449 | — |
| 反応物 | Chloromethyl methyl sulfide | HCID 16916 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2,4-Dichloro-1-methylsulfanylmethoxy-benzene | HCID 68577897 | 124.2% |
反応手順
To a solution of 2,4-dichloro-phenol (10 g, 61.35 mmol) in dry DMF (100 mL) was added NaH (2.06 g, 85.89 mmol, 60% in mineral oil). The mixture was stirred for 30 min. at room temperature followed by dropwise addition of chloro-methylsulfanyl-methane (5.65 mL, 67.48 mmol) and stirring was continued for 16 hrs at ambient temperature. The reaction was quenched by addition of water (150 mL) and extracted with diethyl ether (2×100 mL). The combined organic phases were washed with saturated aq. ammonium chloride (2×100 mL), dried (Na2SO4), filtered and evaporated in vacuo afforded 17 g crude 2,4-dichloro-1-methylsulfanylmethoxy-benzene which was used without further purification in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08383683B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-68fb43f11c394765b18bc480b9bf90e0 |
| 出典メモ | uspto-grants-2013_02 |