丁二酸酐 → 4-(3,4-二氟苯基)-4-氧代丁酸

HRID 2257874

反应方程式

HRID 2257874 反应方程式
[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]

参与物

5

反应物 3

HCID 7922丁二酸酐HCID 97061,2-二氟苯HCID 6451240三氯化铝

产物 1

HCID 27583374-(3,4-二氟苯基)-4-氧代丁酸收率 31.2%

试剂、催化剂与溶剂 1

HCID 313海萝胶溶剂

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-403d1ad0902b425aacaf9d3fa1478713
来源数据集
uspto-grants-1997_08
专利号
US05658920

关联笔记

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