Toluene → HCID 22352715, 화합물

HRID 567636

반응식

HRID 567636 반응식
[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]

참가 물질

6

반응물 3

HCID 1140Toluene2회HCID 696191,1,2,2-Tetrahydroperfluoro-1-decanolHCID 79177tert-Butyl bromoacetate

생성물 1

HCID 22352715HCID 22352715, 화합물

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 14797Potassium Hydroxide용매

반응 조건

온도
0 °C

실험 절차

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/dichlormethane/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 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/dichlormethane/acetone=20/10/1)

출처 및 근거

ORD 기록
ord-31ecd48878a447e99291e5f76dbbc009
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06180113B2

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