Methanol → 1H-Perfluorohexane

HRID 53414

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HRID 53414 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

HCID 677301H-Perfluorohexane수율 92.2%

시약·촉매·용매 2

HCID 11332432Hastelloy C촉매HCID 962Water용매

반응 조건

온도
55 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-54f8a64d08b74411b846a4c35d500602
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05618986

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