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Methanol → 1H-Perfluorohexane

HRID 53415
ノート
印刷プレビュー

反応式

HRID 53415 の反応式
CO.[OH-].[K+].[C:5](I)([C:8]([C:11]([C:14]([C:17]([C:20]([F:23])([F:22])[F:21])([F:19])[F:18])([F:16])[F:15])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6]>[Br-].C([P+](CCCC)(CCCC)CCCC)CCC.O>[CH:5]([C:8]([C:11]([C:14]([C:17]([C:20]([F:21])([F:22])[F:23])([F:18])[F:19])([F:15])[F:16])([F:13])[F:12])([F:10])[F:9])([F:7])[F:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 887MethanolHCID 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 98.1%

試薬・触媒・溶媒 2

HCID 76564Tetrabutylphosphonium bromide触媒HCID 962Water
溶媒

実験手順

Into a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel and a thermometer, 200 cc of methanol, 74.3 g (1.1 mols) of 85% potassium hydroxide and 1 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 the dropwise addition, heating and refluxing were continued for tow hours. The conversion at that time was 98.1%. The heating and refluxing were further continued for two hours. Then, the reactor was cooled to room temperature, and 200 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 with 300 g of water to recover the fluorocarbon. Thus, 157 g of C6F13H having a purity of 99.1%, was obtained.

後処理

  1. customInto a 1 l four-necked flask equipped with a stirrer, a reflux condenser, a dropping funnel
  2. temperatureThe reactor was heated
  3. customto 60° C
  4. additionAfter completion of the dropwise addition
  5. temperatureheating
  6. temperaturerefluxing
  7. temperatureThe heating and refluxing
  8. waitwere further continued for two hours
  9. dissolutionto dissolve
  10. customprecipitated potassium iodide
  11. customThe crude reaction solution
  12. customwas separated into two layers
  13. washthe fluorocarbon layer (lower layer) was further washed with 300 g of water
  14. customto recover the fluorocarbon

出典と根拠

ORDレコード
ord-21a112d1251042d38557af52c999c171
出典データセット
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05618986

反応ノート

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