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Hydrochloric Acid → 1,1,1,3,3,3-Hexafluoro-2,2-bis[4-(methylsulfonyloxy)phenyl]propane

HRID 1086325
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HRID 1086325 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH:6]1[C:11]([C:12]([C:24]([F:27])([F:26])[F:25])([C:20]([F:23])([F:22])[F:21])[C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=2)=[CH:10][CH:9]=[C:8]([OH:28])[CH:7]=1.Cl>N1C=CC=CC=1>[S:2]([O:19][C:16]1[CH:15]=[CH:14][C:13]([C:12]([C:11]2[CH:10]=[CH:9][C:8]([O:28][S:2]([CH3:1])(=[O:4])=[O:3])=[CH:7][CH:6]=2)([C:24]([F:25])([F:26])[F:27])[C:20]([F:23])([F:22])[F:21])=[CH:18][CH:17]=1)([CH3:1])(=[O:4])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 31297Methanesulfonyl chlorideHCID 73864bisphenol AF

생성물 1

HCID 142050441,1,1,3,3,3-Hexafluoro-2,2-bis[4-(methylsulfonyloxy)phenyl]propane수율 82%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

11.8 g (0.1 mol) of methanesulfonyl chloride are added dropwise, at a reaction temperature of 0-5° C., to a solution of 16.8 g (0.05 mol) of bisphenol AF in 100 ml of pyridine. Stirring is then continued for a further hour at 5° C. and overnight at room temperature. The reaction mixture is then acidified with sufficient half-concentrated hydrochloric acid to precipitate the product. Filtering off with suction and washing with water gives 24 g of crude product, and recrystallization from toluene gives 20.2 g (82% yield) of 2,2-bis-(4-mesyloxyphenyl)-hexafluoropropane are isolated. M.p 136-138° C.

후처리

  1. customto precipitate the product
  2. filtrationFiltering off with suction
  3. washwashing with water
  4. customgives
  5. custom24 g of crude product, and recrystallization from toluene

출처 및 근거

ORD 기록
ord-a3bcef01aadb4098b0aa8f49542f135f
출처 데이터셋
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05028728

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