Réaction #76214

ord-3bf23ac72d0e454e87c0e21c7a1e4332

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurewas heated
  2. 2
    Températureunder reflux
  3. 3
    ConcentrationThe reaction mixture was concentrated
  4. 4
    workup.ADDITIONpoured into water (1 L)
  5. 5
    FiltrationThe precipitated solid was collected by filtration
  6. 6
    Lavagewashed with water
  7. 7
    Séchagewith isopropyl ether, air-dried
  8. 8
    Autrefurther dried under reduced pressure at 40° C.

Mode opératoire

A mixture of 2-bromo-3′,4′-dichloroacetophenone (78.0 g), sodium formate (68.0 g) and methanol (300 mL) was heated under reflux and stirred for 16 h. The reaction mixture was concentrated and poured into water (1 L). The precipitated solid was collected by filtration, washed with water and then with isopropyl ether, air-dried, and further dried under reduced pressure at 40° C. to give the title compound as crystals (25.0 g, 42%). Recrystallization from ethyl acetate-hexane gave pale-yellow prism crystals. melting point: 115-118° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06699995B1uspto-grants-2004_03