関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-Chloro-1,1,1-trifluoroethane | HCID 6408 | — |
| 反応物 | Benzyl mercaptan | HCID 7509 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 触媒 | Hexadecyltributylphosphonium bromide | HCID 84716 | — |
| 生成物 | Benzyl 2,2,2-trifluoroethyl sulfide | HCID 2737790 | 84% |
反応手順
A mixture of 1-chloro-2,2,2-trifluoroethane (20 g), benzyl mercaptan (12.4 g, 99% strength), sodium hydroxide (22.0 g of a 22% aqueous solution) and hexadecyl tributyl phosphonium bromide (0.51 g) was charged to a resealable Carius tube under a nitrogen atmosphere and heated at 70° C. for 10 hours. The tube was then cooled to 0° C., unsealed and the contents separated into two layers. The lower organic layer was collected, washed with water and purified by short path distillation to give 2,2,2-trifluoroethylthiomethylbenzene, b.p. 60°-70° C./ 10 mmHg, 17.4 g (yield 84%, strength 99%). The identity of the product was confirmed by gc-mass spectroscopy and nuclear magnetic reconance, and by comparison with data provided in C. Bunyagidj et al, J Org. Chem., 1981, 46 3335.
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-3a7efd3878424318b295329d78bcf8e4 |
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| 出典メモ | uspto-grants-1993_11 |
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