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Methanol → 1H-Perfluorohexane

HRID 53415
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HRID 53415 반응식
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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

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

생성물 1

HCID 677301H-Perfluorohexane수율 98.1%

시약·촉매·용매 2

HCID 76564Tetrabutylphosphonium bromide촉매HCID 962Water
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-21a112d1251042d38557af52c999c171
출처 데이터셋
uspto-grants-1997_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05618986

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