関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | tert-Butyl mercaptan | HCID 6387 | — |
| 反応物 | 1,2,4,5-Tetrachlorobenzene | HCID 7270 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1,2,4,5-Tetrakis(tert-butylthio)benzene | HCID 11812054 | 69% |
反応手順
Sodium (9.3 g, 0.18 mol) was added to a degassed solution of 2-methyl-2-propanethiol (20.9 mL, 0.18 mol) in dry DMF (105 mL), under stirring at 0° C. in nitrogen atmosphere. The mixture was allowed to reach room temperature (RT, 20-25° C.) and stirred overnight. 1,2,4,5-Tetrachlorobenzene (8.0 g, 0.037 mol) was then added and the resulting mixture was stirred at RT for 2 h and then gently refluxed for 18 h. After cooling at RT, the reaction mixture was poured over ice (100 g), the precipitate was removed by filtration, washed with water, and dried to give 11.0 g of the title compound as an off-white powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09381257B2 |
|---|
| 出典データセット | uspto-grants-2016_07 |
|---|
| ORD ID | ord-87b806a754504fe39d1e651f26080e47 |
|---|
| 出典メモ | uspto-grants-2016_07 |
|---|