1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane → 1H-Perfluorohexane

HRID 53420

反応式

HRID 53420 の反応式
CC(C)([O-])C.[K+].[C:7](I)([C:10]([C:13]([C:16]([C:19]([C:22]([F:25])([F:24])[F:23])([F:21])[F:20])([F:18])[F:17])([F:15])[F:14])([F:12])[F:11])([F:9])[F:8]>>[CH:7]([C:10]([C:13]([C:16]([C:19]([C:22]([F:23])([F:24])[F:25])([F:20])[F:21])([F:17])[F:18])([F:15])[F:14])([F:12])[F:11])([F:9])[F:8]

参加物

3

反応物 2

HCID 677331,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexaneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 677301H-Perfluorohexane収率 94.4%

実験手順

Into a 1 l four-necked flask equipped with a stirrer, a distillation apparatus-equipped reflux condenser, a dropping funnel and a thermometer, 400 cc of isopropyl alcohol (the water content in the isopropyl alcohol being not higher than 50 ppm, the same is true in the following Examples), and 84.2 g (0.75 mol) of potassium tert-butoxide 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 two hours. After completion of the dropwise addition, heating and refluxing were continued for one hour. The conversion at that time was 100%. A fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor and further washed five times with 200 g of water, to obtain 151 g of C6F13H having a purity of 99.8%. In the reactor, no formation of tar was observed.

後処理

  1. customInto a 1 l four-necked flask equipped with a stirrer
  2. distillationa distillation
  3. customapparatus-equipped
  4. temperaturereflux condenser, a dropping funnel
  5. additionwere charged
  6. temperatureThe reactor was heated
  7. customto 60° C
  8. additionAfter completion of the dropwise addition
  9. temperatureheating
  10. temperaturerefluxing
  11. waitwere continued for one hour
  12. distillationA fraction with a boiling point of up to 75° C. was recovered by distillation from the reactor
  13. washfurther washed five times with 200 g of water

出典と根拠

ORDレコード
ord-10f61eec01514446b12ab54de9e82bc4
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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