関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Mercaptopropionic Acid | HCID 6514 | — |
| 反応物 | 2,6-Di-tert-butyl-4-methylpyridine | HCID 98898 | — |
| 反応物 | Pentafluoroethylphenyliodonium trifluoromethanesulfonate | HCID 11488264 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 178526190 | HCID 178526190 | — |
反応手順
2.0 ml of methylene chloride, 0.05 ml (0.58 mmol) of 3-mercaptopropionic acid and 120 mg (0.59 mmol) of 2,6-di-tert-butyl-4-methylpyridine were charged in a flask, and 261 mg (0.55 mmol) of pentafluoroethylphenyliodonium trifluoromethanesulfonate was added thereto in small portions while stirring at room temperature, followed by stirring the mixture at room temperature for 20 minutes. The resulting white precipitate was filtered, subjected to column chromatography of a small amount of silica gel and, after eluting iodobenzene with hexane, the desired product was eluted with diethyl ether. Diethyl ether was distilled off from the eluate to obtain 3-pentafluoroethylthiopropionic acid as a colorless liquid. A sample of the product was purified by gas chromatography. Yield, 83%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04371710 |
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| 出典データセット | uspto-grants-1983_02 |
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| ORD ID | ord-071eaa1c832b47528a922645f141246c |
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| 出典メモ | uspto-grants-1983_02 |
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