関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-(2-Iodo-benzyl)-isothiourea | HCID 23089112 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Iodo-2-[(methylthio)methyl]-benzene | HCID 10061336 | 89% |
反応手順
To a mixture of 2-(2-iodo-benzyl)-isothiourea (13.53 g, 36.2 mmol) from previous step and a solution of NaOH (22 mL) in water (15 mL) was added dropwise dimethylsulfate (4.1 mL, 43.4 mmol). The reaction mixture was heated to reflux (105° C.) for 2 h, cooled. The resulting oil was then extracted into diethyl oxyde, the organic layer was washed with water, dried over Na2SO4. On concentration the solution generated a yellow oil that was directly used in the next step without any further purification (8.5 g, yield=89%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07981907B2 |
|---|
| 出典データセット | uspto-grants-2011_07 |
|---|
| ORD ID | ord-1e3f097074eb43ca8f36850b5f394187 |
|---|
| 出典メモ | uspto-grants-2011_07 |
|---|