HRID325863

反应详情

EQUATION

反应方程式

HRID 325863 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a corresponding manner was made 3-bromo-6-fluoro-1-indanone melting at 62-64 degrees Centigrade, and 3-bromo-5-fluoro-1-indanone melting at 44-47 degrees Centigrade. To a solution of 113 grams of 3-bromo-6-chloro-1-indanone in 1400 milliliters of dry benzene were added over 10 minutes 230 grams of aluminiumchloride in portions. The reaction mixture was then refluxed for 3 hours, cooled and treated with crushed ice and concentrated hydrochloric acid. The organic phase was separated and extracted with 1 N sodium hydroxide and water, dried over anhydrous magnesium sulfate, treated with active carbon and concentrated in vacuo. The residue was taken up to 450 milliliters of hot n-hexane, cooled and filtered to give 96 grams of 3-phenyl-6-chloro-1-indanone melting at 84-92 degrees Centigrade.

WORKUP

后处理

  1. temperatureThe reaction mixture was then refluxed for 3 hours
  2. temperaturecooled
  3. customThe organic phase was separated
  4. extractionextracted with 1 N sodium hydroxide and water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. additiontreated with active carbon
  7. concentrationconcentrated in vacuo
  8. temperaturecooled
  9. filtrationfiltered