反応 #1328421

ord-284ab8b931e540ada41736c24d6676e3

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.DISTILLATIONThe solvent was distilled off
  2. 2
    抽出the mixture was extracted with diethyl ether
  3. 3
    ろ過the resulting precipitate was filtered off with suction
  4. 4
    その他dried

実験手順

179.5 g (1.3 mol) of potassium carbonate and, a little at a time, 94.5 g (0.62 mol) of 3-bromopropionic acid were added to a solution of 125.4 g (0.62 mol) of methyl 2-mercapto-4-chlorobenzoate in 1.5 l of acetone, and the reaction mixture was stirred at room temperature for 12 hours. The solvent was distilled off, the residue was taken up in water and the mixture was extracted with diethyl ether. The aqueous phase was then made acidic using concentrated hydrochloric acid, and the resulting precipitate was filtered off with suction and dried. This gave 150 g (88%) of methyl 2-(2-hydroxycarbonyleth-1-yl)thio-4-chlorobenzoate.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07115545B1uspto-grants-2006_10