Toluene → HCID 22352715、化合物

HRID 1764985

反応式

HRID 1764985 の反応式
[C:1]([O:5][C:6](=[O:9])[CH2:7]Br)([CH3:4])([CH3:3])[CH3:2].[CH2:10]([C:13]([F:37])([F:36])[C:14]([F:35])([F:34])[C:15]([F:33])([F:32])[C:16]([F:31])([F:30])[C:17]([F:29])([F:28])[C:18]([F:27])([F:26])[C:19]([F:25])([F:24])[C:20]([F:23])([F:22])[F:21])[CH2:11][OH:12].C1(C)C=CC=CC=1>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.[OH-].[K+]>[C:1]([O:5][C:6](=[O:9])[CH2:7][O:12][CH2:11][CH2:10][C:13]([F:36])([F:37])[C:14]([F:34])([F:35])[C:15]([F:32])([F:33])[C:16]([F:30])([F:31])[C:17]([F:28])([F:29])[C:18]([F:26])([F:27])[C:19]([F:25])([F:24])[C:20]([F:23])([F:22])[F:21])([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 3

HCID 1140Toluene2 回HCID 696191,1,2,2-Tetrahydroperfluoro-1-decanolHCID 79177tert-Butyl bromoacetate

生成物 1

HCID 22352715HCID 22352715、化合物

試薬・触媒・溶媒 2

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 14797Potassium Hydroxide溶媒

反応条件

温度
0 °C

実験手順

10.51 g (53.9 mmol) of bromoacetic acid-tert-butyl ester is added in drops to a mixture of 10 g (21.55 mmol) of 1H,1H,2H,2H-perfluorodecan-1-ol and 0.73 g (2.15 mmol) of tetrabutylammonium hydrogen sulfate in 100 ml of 60% potassium hydroxide solution/50 ml of toluene while being stirred vigorously at 0° C. It is stirred for 1 hour at 0° C. 200 ml of toluene is added, the aqueous phase is separated and extracted twice with 50 ml of toluene each. The combined organic phases are dried on magnesium sulfate and concentrated by evaporation in a vacuum. The residue is chromatographed on silica gel (mobile solvent: hexane/dichloromethane/acetone=20/10/1).

後処理

  1. stirringIt is stirred for 1 hour at 0° C
  2. customthe aqueous phase is separated
  3. extractionextracted twice with 50 ml of toluene each
  4. customThe combined organic phases are dried on magnesium sulfate
  5. concentrationconcentrated by evaporation in a vacuum
  6. customThe residue is chromatographed on silica gel (mobile solvent: hexane/dichloromethane/acetone=20/10/1)

出典と根拠

ORDレコード
ord-c4f4165d5e1f4a9a8af967a130849eec
出典データセット
uspto-grants-2007_06
特許番号
US07226578B2

関連ノート

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