関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Bromo-1,1,1-trifluoroethane | HCID 67898 | — |
| 反応物 | Sodium sulfide nonahydrate | HCID 73972 | — |
| 反応物 | Sulfur | HCID 5362487 | — |
| 触媒 | Hexadecyltributylphosphonium bromide | HCID 84716 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Bis(trifluoroethyl)dithio | HCID 15036106 | — |
反応手順
A mixture of 2,2,2-trifluoroethyl bromide (9.8 g), sodium sulphide nonahydrate (14.4 g), sulphur (1.9 g), hexadecyl tributyl phosphonium bromide (1.0 g) and water (18.0 g) was charged to a Carius tube under a nitrogen atmosphere and the tube sealed. The tube was heated to 70° C. for 8 hours, cooled and the contents subjected to steam distillation to give bis-(2,2,2-trifluoroethyl) disulphide as an oil in a yield of 67° C. The product was identified by GC-mass spectroscopy.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05258547 |
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| 出典データセット | uspto-grants-1993_11 |
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| ORD ID | ord-70a8131d2c2242bda19952751b86f54d |
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| 出典メモ | uspto-grants-1993_11 |
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