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 | 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 | Hastelloy C | HCID 11332432 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1H-Perfluorohexane | HCID 67730 | 93% |
反応手順
Into a 20 l Hastelloy C autoclave equipped with a stirrer, a reflux condenser and a thermometer, 5130 g of methanol and 60 g of isopropyl alcohol and 1485 g (22.5 mols) of 85% potassium hydroxide were charged. The reactor was heated to bring the internal temperature to 50° C. Then, 4460 g (10 mols) of C6F13I was fed thereto over a period of two hours. While maintaining the internal temperature of the reactor at a level of from 50° to 55° C. stirring was continued for 10 hours. The conversion was more than 99.9%. The reactor was cooled to room temperature, and then, 3200 g of water was added to dissolve precipitated potassium iodide. The crude reaction solution was separated into two layers, and the fluorocarbon layer (lower layer) was further washed twice with 3200 g of water to obtain 2975 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 |
|---|
| 特許番号 | US05618986 |
|---|
| 出典データセット | uspto-grants-1997_04 |
|---|
| ORD ID | ord-a39525dfa9c34ad0ae8e59b487ad02c5 |
|---|
| 出典メモ | uspto-grants-1997_04 |
|---|