Dimethyl Sulfoxide → 1,3-Bis(4-formylphenoxy)-5-chlorobenzene

HRID 263530

반응식

HRID 263530 반응식
F[C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.[Cl:10][C:11]1[CH:12]=[C:13]([OH:18])[CH:14]=[C:15]([CH:17]=1)[OH:16].[C:19](=[O:22])([O-])[O-].[K+].[K+].CS(C)=O>C(OCC)(=O)C.O>[CH:6]([C:5]1[CH:8]=[CH:9][C:2]([O:16][C:15]2[CH:17]=[C:11]([Cl:10])[CH:12]=[C:13]([O:18][C:2]3[CH:9]=[CH:8][C:5]([CH:19]=[O:22])=[CH:4][CH:3]=3)[CH:14]=2)=[CH:3][CH:4]=1)=[O:7]

참가 물질

7

반응물 4

HCID 679Dimethyl SulfoxideHCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 945541,3-Benzenediol, 5-chloro-

생성물 1

HCID 190384981,3-Bis(4-formylphenoxy)-5-chlorobenzene수율 32%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

반응 조건

온도
100 °C

실험 절차

p-Fluorobenzaldehyde (7.7 g), 5.9 g of 5-chlororesorcinol and 12.3 g of anhydrous potassium carbonate were added to 50 ml of dimethyl sulfoxide and stirred for 12 hours at 100° C. After completion of the reaction, 100 ml of water and 200 ml of ethyl acetate were added to carry out phase separation. After three times of washing with 50 ml of 10% sodium chloride aqueous solution and subsequent drying over anhydrous magnesium sulfate, the solvent was evaporated. The resulting oily material was subjected to silica gel column chromatography (hexane:ethyl acetate (7:1)) to obtain 3.5 g of 1,3-bis(4-formylphenoxy)-5-chlorobenzene.

후처리

  1. additionwere added
  2. customphase separation
  3. washAfter three times of washing with 50 ml of 10% sodium chloride aqueous solution
  4. dry with materialsubsequent drying over anhydrous magnesium sulfate
  5. customthe solvent was evaporated

출처 및 근거

ORD 기록
ord-e01cc9ccd90348c2825383fc5f394d19
출처 데이터셋
uspto-grants-1997_07
특허 번호
US05643931

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