関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Diethyl Ether | HCID 3283 | — |
| 反応物 | Pentafluorobenzene | HCID 9696 | — |
| 反応物 | CID 53628100 | HCID 178418400 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 生成物 | HCID 178419089 | HCID 178419089 | — |
反応手順
Inside of a 100 ml volume glass three-neck flask equipped with a 50 ml volume glass dropping funnel, temperature resistor and septum rubber was sufficiently replaced with nitrogen. Into the flask, 5 g (29.8 mmol) of pentafluorobenzene and 30 ml of diethyl ether were charged, of which solution was cooled to -65° C. Thereafter, 12.3 g (29.8 mmol) of 16.1 wt. % hexane solution of sec-butyllithium charged into the dropping funnel were added dropwise while making the inner temperature not to exceed -55° C. After the completion of dropwise addition, the reaction mixture was kept at a temperature of -65°~-55° C. with stirring to give pentafluorophenyllithium. The yield of pentafluorobenzoic acid obtained by blowing of carbon dioxide into the prepared solution of pentafluorophenyllithium was 96.8% by means of gas chromatographic quantitative determination.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05387727 |
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| 出典データセット | uspto-grants-1995_02 |
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| ORD ID | ord-fe38548d76074eefa9690be6358af741 |
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| 出典メモ | uspto-grants-1995_02 |
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