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

HRID 263530

反応式

HRID 263530 の反応式
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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e01cc9ccd90348c2825383fc5f394d19
出典データセット
uspto-grants-1997_07
特許番号
US05643931

関連ノート

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