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Methanol → 1H-Perfluorohexane

HRID 53412
ノート
印刷プレビュー

反応式

HRID 53412 の反応式
CO.C(O)(C)C.[OH-].[Na+].[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]>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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 3776IsopropanolHCID 14798Sodium 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 90.6%

試薬・触媒・溶媒 1

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, 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.

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. waitwere continued for 6 hours
  8. dissolutionto dissolve
  9. customprecipitated sodium iodide
  10. customThe crude reaction solution
  11. customwas separated into two layers
  12. washthe fluorocarbon layer (lower layer) was further washed twice with 300 g of water

出典と根拠

ORDレコード
ord-516c4e4d90434ed7a6d5c51931e5f15b
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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