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Sodium Sulfide → Bis(2,6-dichlorobenzyl) sulfide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Sulfide | HCID 14804 | — |
| 反応物 | 2,6-Dichlorobenzyl chloride | HCID 74832 | — |
| 触媒 | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Bis(2,6-dichlorobenzyl) sulfide | HCID 20404720 | 80.4% |
反応手順
A mixture of 98.8 g (0.411 mol) of sodium sulfide, 5.0 g of tetrabutylammonium hydrogen sulfate and 110 ml of water are stirred in a reaction vessel equipped with a stirrer, thermometer and heatable dropping funnel, until a solution is obtained. 107.2 g of melted 2,6-dichlorobenzyl chloride are added with vigorous stirring over a period of 25 minutes at such a rate that the inside temperature does not exceed 55° C. The reaction mixture is worked up as in Example 9a) to give 77.6 g (80% of theory) of bis(2,6-dichlorobenzyl) sulfide in the form of white crystals of melting point 128°-130° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05247113 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-36a943ae44634d7499c53401c1d522ef |
| 出典メモ | uspto-grants-1993_09 |