関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane | HCID 67733 | — |
| 触媒 | Tetrabutylphosphonium bromide | HCID 76564 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1H-Perfluorohexane | HCID 67730 | 93.1% |
反応手順
Into a 1 l four-necked flask equipped with a stirrer, a distillation apparatus-equipped refluxing condenser, a dropping funnel and a thermometer, 200 cc of methanol, 131 g of (1.1 mols) of 48% potassium hydroxide and 3 g of tetrabutylphosphonium bromide were charged. The reactor was heated to bring the internal temperature to 60° C. Then, 223 g (0.5 mol) of C6F13I was dropwise added thereto over a period of one hour. After completion of dropwise addition, heating and refluxing were continued for two hours. The conversion at that time was 97.0%. A fraction with a boiling point of up to 60° C. was recovered by distillation from the reactor. The recovered liquid was washed with 300 g of water to recover the fluorocarbon. Thus, 149 g of C6F13H having a purity of 99.9%, was obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05618986 |
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| 出典データセット | uspto-grants-1997_04 |
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| ORD ID | ord-58ac287d8cc14b7892f4b6e9a504f375 |
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| 出典メモ | uspto-grants-1997_04 |
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