関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Isopropanol | HCID 3776 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane | HCID 67733 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1H-Perfluorohexane | HCID 67730 | 90.6% |
反応手順
Into a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 256 g of methanol, 3 g of isopropyl alcohol and 46.4 g (1.16 mol) of sodium hydroxide 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 the dropwise addition, heating and refluxing were continued for 6 hours. The conversion was more than 99.9%. The reactor was cooled to room temperature, and then, 300 g of water was added to dissolve precipitated sodium iodide. The crude reaction solution was separated into two layers, and the fluorocarbon layer (lower layer) was further washed twice with 300 g of water to obtain 145 g (purity: 99.9%) of C6F13H. In the reactor, no formation of tar was observed.
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-516c4e4d90434ed7a6d5c51931e5f15b |
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| 出典メモ | uspto-grants-1997_04 |
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