Реакция #461800

Уравнение реакции

sodium percarbonate

3,4-difluorobenzophenone

→

3,4-difluorobenzoic acid

Выход 95.5%

Растворители

trifluoroacetic acid

Условия реакции

Обработка

1. 1
   Другоеto rise to 20° C
2. 2
   workup.ADDITIONwere then added
3. 3
   ЭкстракцияThe mixture was subsequently extracted twice with dichloromethane
4. 4
   Промывкаthe organic phases were washed (NaHCO3) until the washings
5. 5
   ДругоеThe solvent was then removed

Методика

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.).

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