Reaktion #832856

ord-b14a83937ea54b66b9bb63b80b93e972

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeA white precipitate quickly formed
  2. 2
    TemperaturThe reaction was heated
  3. 3
    Temperaturto reflux for 24 hours
  4. 4
    TemperaturUpon cooling
  5. 5
    Extraktionextracted twice with methylene chloride (25 ml@)
  6. 6
    WaschenThe combined organic extracts were successively washed with 5% sodium hydroxide and brine solutions

Vorschrift

To a stirred solution of 5-[2-chloro-4-(trifluoromethyl)phenoxy]-2-nitrobenzyl chloride (3.8 g, 0.01 mole) in acetone (10 ml) was successively added diethyl DL malate (1.9 g, 0.01 mole) in acetone (10 ml) and triethylamine (1.01 g, 0.01 mole) in acetone (5 ml). A white precipitate quickly formed. The reaction was heated to reflux for 24 hours. Upon cooling, the reaction was poured in water (75 ml) and extracted twice with methylene chloride (25 ml@). The combined organic extracts were successively washed with 5% sodium hydroxide and brine solutions. The dried solution was stripped of solvent to give 3.5 g of an amber oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04599442uspto-grants-1986_07