Sodium percarbonate → 3,4-Difluorobenzoic acid

HRID 374618

反応式

HRID 374618 の反応式
[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]

参加物

4

反応物 2

HCID 159762Sodium percarbonateHCID 5699083,4-Difluorobenzophenone

生成物 1

HCID 991663,4-Difluorobenzoic acid収率 95.5%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-3a540bda32044b3891e823049d0d41e1
出典データセット
uspto-grants-1996_01
特許番号
US05481032

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