関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Pentafluorophenol | HCID 13041 | — |
| 反応物 | Phosphorus pentachloride | HCID 24819 | — |
| 反応物 | alpha-Cyanobenzeneacetic acid | HCID 26403 | — |
| 溶媒 | Carbon Tetrachloride | HCID 5943 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | alpha-Cyano-phenylacetic acid pentafluorophenyl ester | HCID 20402416 | — |
反応手順
8 g. (0.05 moles) of α-cyano-phenylacetic acid are dissolved in 80 ml. of dichloromethane. 10.2 g. (0.05 moles) of phosphorus pentachloride are added and the mixture is stirred for two hours at the boiling point of dichloromethane. The solvent is distilled off and the residue is taken up in carbontetrachloride and the solution is added dropwise to 9.2 g. (0.05 moles) of pentafluorophenol and 4 ml. (0.05 moles) of pyridine-dissolved in 200 ml. of carbontetrachloride. The reaction mixture is cooled to 0° C. and the pyridine chlorohydrate is washed with 2n hydrochloride acid. The organic layer is washed twice with 40 ml. of water, dried over magnesium sulfate and evaporated. The α-cyano-phenylacetic acid-pentafluorophenyl ester is recrystallized from petrolether
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04508658 |
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| 出典データセット | uspto-grants-1985_04 |
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| ORD ID | ord-b008978120024e89b3f15211d4f30f88 |
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| 出典メモ | uspto-grants-1985_04 |
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