Реакция #321758

ord-8dcf205b41c142fa875fb34c962140db

Уравнение реакции

Cl
hydrochloric acid
O=C(O)c1ccc(O)cc1F
2-fluoro-4-hydroxybenzoic acid
[K+].[OH-]
potassium hydroxide
CC(=O)OC(C)=O
acetic anhydride
CC(=O)Oc1ccc(C(=O)O)c(F)c1
2-fluoro-4-acetoxybenzoic acid
Выход 62.4%

Растворители

Условия реакции

Температура
0°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    workup.DISSOLUTIONdissolved
  2. 2
    workup.STIRRINGAfter stirring
  3. 3
    Другоеto precipitate a crystal
  4. 4
    ФильтрацияThe crystal was recovered by filtration
  5. 5
    Промывкаby washing with water
  6. 6
    Другоеdrying

Методика

In a 100 ml-reaction vessel, 12.1 g (1.83×10-1M) of potassium hydroxide and 50 ml of water were placed, followed by cooling to 0° C. To the mixture, 12.0 g (7.69×10-2M) of 2-fluoro-4-hydroxybenzoic acid was added and dissolved therein. To the solution, 7.9 g (7.74×10-2M) of acetic anhydride was added dropwise in 30 minutes at 0° C., followed by stirring for 2 hours. After stirring, the reaction mixture was acidified with 6N-hydrochloric acid to precipitate a crystal. The crystal was recovered by filtration, followed by washing with water and drying to obtain 9.5 g of 2-fluoro-4-acetoxybenzoic acid (Yield: 62.4%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05595685uspto-grants-1997_01