Methanol → 1H-Perfluorohexane

HRID 53414

反応式

HRID 53414 の反応式
CO.C(O)(C)C.[OH-].[K+].[C:9](I)([C:12]([C:15]([C:18]([C:21]([C:24]([F:27])([F:26])[F:25])([F:23])[F:22])([F:20])[F:19])([F:17])[F:16])([F:14])[F:13])([F:11])[F:10]>[Cr].[Co].O>[CH:9]([C:12]([C:15]([C:18]([C:21]([C:24]([F:25])([F:26])[F:27])([F:22])[F:23])([F:19])[F:20])([F:17])[F:16])([F:14])[F:13])([F:11])[F:10]

参加物

7

反応物 4

HCID 887MethanolHCID 3776IsopropanolHCID 14797Potassium HydroxideHCID 677331,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane

生成物 1

HCID 677301H-Perfluorohexane収率 92.2%

試薬・触媒・溶媒 2

HCID 11332432Hastelloy C触媒HCID 962Water溶媒

反応条件

温度
55 °C

実験手順

Into a 20 l Hastelloy C autoclave equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 7700 g of methanol, 60 g of isopropyl alcohol and 1980 g (30 mols) of 85% potassium hydroxide were charged. The reactor was heated to bring the internal temperature to 55° C. Then, 4460 g (10 mols) of C6F13I was fed thereto over a period of two hours. While maintaining the reactor at 55° C. stirring was continued for 10 hours. The conversion was more than 99.9%. 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 2951 g of C6F13H (purity: 99.9%, 3.9 ppm of C6F13I was detected). In the reactor, no formation of tar was observed.

後処理

  1. temperatureThe reactor was heated
  2. customto 55° C
  3. waitwas continued for 10 hours
  4. dissolutionto dissolve
  5. customprecipitated potassium iodide
  6. customThe crude reaction solution
  7. customwas separated into two layers
  8. washthe fluorocarbon layer (lower layer) was further washed twice with 3200 g of water

出典と根拠

ORDレコード
ord-54f8a64d08b74411b846a4c35d500602
出典データセット
uspto-grants-1997_04
特許番号
US05618986

関連ノート

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