関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | 2,6-Dichlorotoluene | HCID 8368 | — |
| 反応物 | Sodium methanethiolate | HCID 4378561 | — |
| 溶媒 | Hexamethylphosphoramide | HCID 12679 | — |
| 生成物 | 1-Chloro-2-methyl-3-(methylthio)benzene | HCID 14801176 | — |
反応手順
200 g (1.24 mol) of 2,6-dichlorotoluene were dissolved in 600 ml of hexamethylphosphoramide and treated with 130.41 g (1.86 mol) of sodium thiomethoxide. The mixture was then heated at 100° C. for 3 h. It was allowed to cool, 88.2 g (0.5 mol) of iodomethane were added and it was stirred at room temperature for 0.5 h. The mixture was then added to 3.5 l of water and extracted with ethyl acetate. The combined organic phases were washed with water, dried over MgSO4 and completely concentrated on a rotary evaporator.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06376429B1 |
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| 出典データセット | uspto-grants-2002_04 |
|---|
| ORD ID | ord-05d9b5bab5de44b5909780c2f67105b6 |
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| 出典メモ | uspto-grants-2002_04 |
|---|
