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Water → 1,1,1,2,2,3,3,4,4-Nonafluoro-8-iodooctane

HRID 1267472
ノート
印刷プレビュー

反応式

HRID 1267472 の反応式
[I-:1].[Na+].CS(O[CH2:8][CH2:9][CH2:10][CH2:11][C:12]([F:24])([F:23])[C:13]([F:22])([F:21])[C:14]([F:20])([F:19])[C:15]([F:18])([F:17])[F:16])(=O)=O.O>CC(C)=O>[I:1][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([F:24])([F:23])[C:13]([F:22])([F:21])[C:14]([F:20])([F:19])[C:15]([F:18])([F:17])[F:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 5238Sodium IodideHCID 120157881-Methanesulfonyloxy-5,5,6,6,7,7,8,8,8-nonafluorooctane

生成物 1

HCID 120157891,1,1,2,2,3,3,4,4-Nonafluoro-8-iodooctane収率 93.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

Sodium iodide (10.32 g, 68.88 mmol) was added to a solution of 1-methanesulfonyloxy-5,5,6,6,7,7,8,8,8-nonafluorooctane (8.5 g, 22.96 mmol) in acetone (300 ml), followed by heating under reflux for 12 hours. After the reaction was completed, water was added to the reaction mixture, which was then extracted twice with ethyl acetate. The combined organic layers were washed with 1% aqueous sodium thiosulfate and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. The solvent was distilled off to give 1-iodo-5,5,6,6,7,7,8,8,8-nonafluorooctane (8.6 g, Yield 93%).

後処理

  1. temperatureby heating
  2. temperatureunder reflux for 12 hours
  3. extractionwas then extracted twice with ethyl acetate
  4. washThe combined organic layers were washed with 1% aqueous sodium thiosulfate and saturated aqueous sodium chloride
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-ed8c2c373927482db1be75d1311ff254
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06552069B1

反応ノート

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