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 | Tetrabutylammonium Bromide | HCID 74236 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | 1H-Perfluorohexane | HCID 67730 | 91.2% |
反応手順
Into a 1 l four-necked flask equipped with a stirrer, a distillation apparatus-equipped reflux condenser, a dropping funnel and a thermometer, 200 cc of isopropyl alcohol, 87.5 g (0.75 mol) of 48% potassium hydroxide and 1 g of tetrabutyl ammonium 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 3 hours. The conversion at that time was 99.9%. A fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor. This recovered liquid was washed five times with 200 g of water, and acetone and isopropyl alcohol were removed. Thus, 146 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-170786d7e07c432a8a0b319eaf4533a6 |
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| 出典メモ | uspto-grants-1997_04 |
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