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Toluene → HCID 15406176, 화합물

HRID 1764986
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HRID 1764986 반응식
[C:1]([O:5][C:6](=[O:9])[CH2:7]Br)([CH3:4])([CH3:3])[CH3:2].[CH2:10]([C:13]([F:25])([F:24])[C:14]([F:23])([F:22])[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17])[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:24])([F:25])[C:14]([F:22])([F:23])[C:15]([F:20])([F:21])[C:16]([F:17])([F:19])[F:18])([CH3:4])([CH3:3])[CH3:2]
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6

반응물 3

HCID 1140Toluene2회HCID 748831-Hexanol, 3,3,4,4,5,5,6,6,6-nonafluoro-HCID 79177tert-Butyl bromoacetate

생성물 1

HCID 15406176HCID 15406176, 화합물

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 14797Potassium Hydroxide
용매

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온도
0 °C

실험 절차

29.54 g (151.5 mmol) of bromoacetic acid-tert-butyl ester is added in drops to a mixture of 20 g (75.73 mmol) of 1H,1H,2H,2H-perfluorohexan-1-ol and 2.57 g (7.57 mmol) of tetrabutylammonium hydrogen sulfate in 300 ml of 60% aqueous potassium hydroxide solution/200 ml of toluene while being stirred vigorously at 0° C. It is stirred for 1 hour at 0° C. 100 ml of toluene is added, the aqueous phase is separated and extracted twice with 50 ml of toluene. 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).

후처리

  1. stirringIt is stirred for 1 hour at 0° C
  2. customthe aqueous phase is separated
  3. extractionextracted twice with 50 ml of toluene
  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)

출처 및 근거

ORD 기록
ord-215f1c6da231493f906efc545ade8d6f
출처 데이터셋
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07226578B2

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