反応 #1591

ord-df91626c72824b1cb4c0c7f9c249511e

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.ADDITIONAfter the addition
  2. 2
    その他was 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
    抽出extracted with methylene chloride (3×150 ml)
  5. 5
    洗浄the combined organic layers were washed with water
  6. 6
    その他dried
  7. 7
    その他evaporated under vacuum

実験手順

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).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05726162uspto-grants-1998_03