Succinic anhydride → 4-(3,4-Difluorophenyl)-4-oxobutanoic acid

HRID 2257874

反応式

HRID 2257874 の反応式
[C:1]1(=[O:7])[O:6][C:4](=[O:5])[CH2:3][CH2:2]1.[Cl-].[Al+3].[Cl-].[Cl-].[F:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=1[F:19]>Cl>[F:12][C:13]1[CH:18]=[C:17]([C:1](=[O:7])[CH2:2][CH2:3][C:4]([OH:6])=[O:5])[CH:16]=[CH:15][C:14]=1[F:19]

参加物

5

反応物 3

HCID 7922Succinic anhydrideHCID 97061,2-DifluorobenzeneHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 27583374-(3,4-Difluorophenyl)-4-oxobutanoic acid収率 31.2%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

45 gm of succinic anhydride and 130.7 gm of aluminum chloride were added to 57 gm of difluorobenzene, and the mixture was heated under reflux for 4 hours. Upon the addition of 200 ml of 1% hydrochloric acid aqueous solution, the reaction mixture was extracted with chloroform, washed with water, and dried over anhydrous sodium sulfate. The solvent was evaporated and the residue was subjected to silica gel column chromatography using a chloroform-methanol (30:1) mixed solvent as an eluant to obtain fractions containing the target compound. The fractions were concentrated to produce 30 gm of the title compound.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 4 hours
  3. extractionthe reaction mixture was extracted with chloroform
  4. washwashed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated
  7. additionmixed solvent as an eluant
  8. customto obtain fractions
  9. additioncontaining the target compound
  10. concentrationThe fractions were concentrated

出典と根拠

ORDレコード
ord-403d1ad0902b425aacaf9d3fa1478713
出典データセット
uspto-grants-1997_08
特許番号
US05658920

関連ノート

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