関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 1,1,1-Trifluoro-4-iodobutane | HCID 2775189 | — |
| 反応物 | Potassium ethanethioate | HCID 23670855 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4,4,4-Trifluorobutyl thioacetate | HCID 86642969 | 97.8% |
反応手順
A mixture of 23.80 g of 1-iodo-4,4,4-trifluorobutane, 100 ml of N,N-dimethylformamide and 11.42 g of potassium thioacetate was heated and stirred at 80° C. for 4 hours under a nitrogen atmosphere. A reaction vessel was cooled in an ice bath. To the reaction mixture was added an aqueous 1N hydrochloric acid solution, and the mixture was extracted with 100 ml of t-butyl methyl ether twice. Organic layers were combined, washed with an aqueous saturated sodium chloride solution, dried over sodium sulfate, filtered, and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 18.20 g of 4,4,4-trifluorobutyl thioacetate represented by the formula:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08247596B2 |
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| 出典データセット | uspto-grants-2012_08 |
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| ORD ID | ord-0e41ff9cecd64e4b89e4f03e0560501c |
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| 出典メモ | uspto-grants-2012_08 |
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