반응 #1591

ord-df91626c72824b1cb4c0c7f9c249511e

반응 방정식

Cc1ccc(C(=O)CCC(=O)O)cc1
3-(4-methylbenzoyl)propionic acid
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum chloride
ClCl
chlorine
Cc1c(Cl)cc(C(=O)CCC(=O)O)cc1Cl
3-(3,5-dichloro-4-methylbenzoyl)propionic acid
수율 44.2%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    기타was bubbled in slowly at 0° C
  3. 3
    workup.ADDITIONAfter 6 hours the reaction mixture was poured into mixture of hydrochloric acid and ice
  4. 4
    추출extracted with methylene chloride (3×150 ml)
  5. 5
    세척the combined organic layers were washed with water
  6. 6
    기타dried
  7. 7
    기타evaporated under vacuum

실험 절차

To a mixture of 3-(4-methylbenzoyl)propionic acid (7.5 g) and methylene chloride (250 ml) was added slowly portionwise aluminum chloride (15 g) at 0° C. After the addition was completed chlorine gas was bubbled in slowly at 0° C. After 6 hours the reaction mixture was poured into mixture of hydrochloric acid and ice and extracted with methylene chloride (3×150 ml), the combined organic layers were washed with water, dried and evaporated under vacuum yielding 3-(3,5-dichloro-4-methylbenzoyl)propionic acid as a yellow solid (4.5 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05726162uspto-grants-1998_03