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

HRID 964687

반응식

HRID 964687 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7e0fd70d0dbc4862ac497b487d494bcb
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05770605

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