Azobisisobutyronitrile → 6,6,7,7,8,8,9,9,9-Nonafluorononan-1-ol

HRID 898089ノート

反応式

HRID 898089 の反応式
CC(N=NC(C#N)(C)C)(C#N)C.I[CH:14]([CH2:19][C:20]([F:32])([F:31])[C:21]([F:30])([F:29])[C:22]([F:28])([F:27])[C:23]([F:26])([F:25])[F:24])[CH2:15][CH2:16][CH2:17][OH:18].P(O)(O)O.C(N(CC)CC)C>O1CCOCC1>[F:31][C:20]([F:32])([C:21]([F:29])([F:30])[C:22]([F:27])([F:28])[C:23]([F:24])([F:25])[F:26])[CH2:19][CH2:14][CH2:15][CH2:16][CH2:17][OH:18]

参加物

6

反応物 4

HCID 6547AzobisisobutyronitrileHCID 8471TriethylamineHCID 107909Phosphorous acidHCID 85830369HCID 85830369、化合物

生成物 1

HCID 154151756,6,7,7,8,8,9,9,9-Nonafluorononan-1-ol

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

A solution of AIBN (4.9 g, 30 mmol) in dioxane (150 cm3) was added dropwise into a solution of 4iodo-6,6,7,7,8,8,9,9,9-nonafluorononan-1-ol (Preparation 1B, 25 g, 58 mmol), phosphorous acid (19.1 g, 0.29 mol) and triethylamine (32.3 g, 0.32 mol) in dioxane (150 cm3) under an atmosphere of nitrogen during reflux. After addition, the reaction mixture was refluxed for a period of time until the GLC analysis revealed a complete reaction (usually an hour). The crude product was extracted into diethyl ether (3×50 cm3) and dried (MgSO4). The solvent was removed in vacuo and the pure product was obtained by reduced pressure distillation as a colourless liquid.

後処理

  1. temperatureduring reflux
  2. additionAfter addition
  3. temperaturethe reaction mixture was refluxed for a period of time until the GLC analysis
  4. customa complete reaction (usually an hour)
  5. extractionThe crude product was extracted into diethyl ether (3×50 cm3)
  6. dry with materialdried (MgSO4)
  7. customThe solvent was removed in vacuo
  8. customthe pure product was obtained by reduced pressure distillation as a colourless liquid

出典と根拠

ORDレコード
ord-20f6b7d6954c4d52918c4cde540dc912
出典データセット
uspto-grants-2008_04
特許番号
US07351452B2

反応ノート

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