反应 #2982

ord-14978e6518ec43e492e5f892cd564bb7

反应方程式

Cl
hydrochloric acid
CCc1ccccc1
ethylbenzene
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum chloride
O=C1CCC(=O)O1
succinic anhydride
CCc1ccc(C(=O)CCC(=O)O)cc1
4-OXO-4-(4-ETHYLPHENYL)BUTYRIC ACID

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The solution is cooled in an ice bath
  2. 2
    workup.STIRRINGThe reaction mixture is stirred for 1 h 30 min at a temperature of 0° C.
  3. 3
    workup.ADDITIONIt is poured into ice
  4. 4
    萃取It is extracted with 3 volumes of ether
  5. 5
    洗涤The organic phases are washed 3 times with 10% potassium carbonate solution
  6. 6
    workup.ADDITIONby adding concentrated hydrochloric acid
  7. 7
    其他The precipitate obtained
  8. 8
    其他recrystallized

实验过程

5 cm3 of ethylbenzene and 2.6 g of aluminum chloride are mixed with magnetic stirring in a 50-cm3 flask. The solution is cooled in an ice bath and 1 g of succinic anhydride is then added. The reaction mixture is stirred for 1 h 30 min at a temperature of 0° C. and then for 3 h at room temperature. It is poured into ice. The resulting mixture is acidified by adding 1N hydrochloric acid (pH 3-4). It is extracted with 3 volumes of ether. The organic phases are washed 3 times with 10% potassium carbonate solution. The aqueous phases are combined and acidified by adding concentrated hydrochloric acid. The precipitate obtained is drained and then recrystallized.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05731352uspto-grants-1998_03