化工社化工社 化学情報印刷レポート · 研究参考用
Sodium sulfide nonahydrate → 4-(4,4-Difluoro-but-3-enyldisulfanyl)-1,1-difluoro-but-1-ene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium sulfide nonahydrate | HCID 73972 | — |
| 反応物 | Sodium disulfide | HCID 89870 | — |
| 反応物 | 4-Bromo-1,1-difluorobut-1-ene | HCID 2782240 | — |
| 反応物 | Sulfur | HCID 5362487 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-(4,4-Difluoro-but-3-enyldisulfanyl)-1,1-difluoro-but-1-ene | HCID 21712911 | — |
反応手順
A solution of sodium disulfide (previously prepared from sodium sulfide nonahydrate (53 g) and sulfur (7.0 g) in ethanol (250 cm3)) was added to 1-bromo4,4-difluorobut-3-ene (50 g) in ethanol (100 cm3). The mixture was gradually heated and stirred under reflux for 2 hours, then cooled and evaporated under reduced pressure. The residue was extracted with diethyl ether, the organic phase filtered to remove sodium bromide and the ether evaporated under reduced pressure to give a liquid which was distilled at 16 mm Hg, bp 120° C. to give the bis-(4,4-difluorobut-3-enyl)disulfide (24 g) as a colourless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06274632B1 |
| 出典データセット | uspto-grants-2001_08 |
| ORD ID | ord-3475dfc603334e56b64100cc5912dc74 |
| 出典メモ | uspto-grants-2001_08 |