过碳酸钠 → 3,4-二氟苯甲酸

HRID 374618

反应方程式

HRID 374618 反应方程式
[C:1]([O-:4])([O-])=[O:2].C([O-])([O-])=O.OO.OO.OO.[Na+].[Na+].[Na+].[Na+].[F:19][C:20]1[CH:21]=[C:22]([CH:31]=[CH:32][C:33]=1[F:34])C(C1C=CC=CC=1)=O>FC(F)(F)C(O)=O>[F:19][C:20]1[CH:21]=[C:22]([CH:31]=[CH:32][C:33]=1[F:34])[C:1]([OH:4])=[O:2]

参与物

4

反应物 2

HCID 159762过碳酸钠HCID 5699083,4-二氟二苯酮

产物 1

HCID 991663,4-二氟苯甲酸收率 95.5%

试剂、催化剂与溶剂 1

HCID 6422三氟乙酸溶剂

实验过程

2.5 g of sodium percarbonate were added over 1 h to a solution of 2.2 g (10 mmol) of 3,4-difluorobenzophenone and 20 ml of trifluoroacetic acid (0° C.) and the temperature was then allowed to rise to 20° C. The mixture was stirred for 16 h at this temperature and 50 g of ice were then added. The mixture was subsequently extracted twice with dichloromethane and the organic phases were washed (NaHCO3) until the washings were neutral. The solvent was then removed. Working-up as described in Example 22 gave 1.2 g (7.6 mmol, 76%) of 3,4-difluorobenzoic acid, which can be obtained analytically pure from water (melting point 113°-120.5° C.).

后处理

  1. customto rise to 20° C
  2. additionwere then added
  3. extractionThe mixture was subsequently extracted twice with dichloromethane
  4. washthe organic phases were washed (NaHCO3) until the washings
  5. customThe solvent was then removed

来源与证据

ORD记录
ord-3a540bda32044b3891e823049d0d41e1
来源数据集
uspto-grants-1996_01
专利号
US05481032

关联笔记

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