HRID22735

反应详情

EQUATION

反应方程式

HRID 22735 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Chloroacetic acid (99.3 mmol, 9.4 g) was added to a suspension of 5-fluoro-2-hydroxy acetophenone (33.1 mmol, 5.1 g) in water (60 mL) containing sodium hydroxide (165.4 mmol, 6.6 g) and the reaction mixture was refluxed for 3.5 hours. The reaction mixture was cooled to room temperature, poured into a separatory funnel and the oily liquid at the bottom of the funnel was discarded. The aqueous top layer was collected, cooled to 0° C. and acidified with conc. HCl. The white precipitate was collected, and air died. The dry solid was crystallized from toluene to obtain (2-acetyl-4-fluoro-phenoxy)-acetic acid, (57%, 4.3 g).

WORKUP

后处理

  1. temperaturethe reaction mixture was refluxed for 3.5 hours
  2. additionpoured into a separatory funnel
  3. customThe aqueous top layer was collected
  4. temperaturecooled to 0° C.
  5. customThe white precipitate was collected
  6. customThe dry solid was crystallized from toluene