HRID35989

反应详情

EQUATION

反应方程式

HRID 35989 的结构方程式

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

In a 250 mL flask equipped with a nitrogen inlet, overhead stirring assembly, and reflux condenser were placed fluorobenzene (117 g, 1.2 mol) and 4-bromobenzoyl chloride (39.8 g, 0.181 mol). The mixture was cooled to 0° C. and aluminum chloride (27 g, 0.20 mol) was added. The mixture was stirred for 15 minutes at 23° C., followed by heating to reflux for 4 h. The reaction was then cooled to 23° C. and stirred for 16 h. The resulting slurry was poured into 2 L of acidic (HCl) water. The organics were extracted with methylene chloride, and dried over magnesium sulfate. The slurry was filtered and the methylene chloride was removed under reduced pressure to yield an off white powder. Recrystallization from ethanol afforded 43.3 g (86%) of 4-bromo-4'-fluorobenzophenone as white crystals: m.p. 106°-107° C., (Lit. 107°-108° C.).

WORKUP

后处理

  1. customIn a 250 mL flask equipped with a nitrogen inlet
  2. temperaturereflux condenser
  3. stirringThe mixture was stirred for 15 minutes at 23° C.
  4. temperatureby heating
  5. temperatureto reflux for 4 h
  6. temperatureThe reaction was then cooled to 23° C.
  7. stirringstirred for 16 h
  8. extractionThe organics were extracted with methylene chloride
  9. dry with materialdried over magnesium sulfate
  10. filtrationThe slurry was filtered
  11. customthe methylene chloride was removed under reduced pressure
  12. customto yield an off white powder
  13. customRecrystallization from ethanol