Reaktion #76214

Reaktionsgleichung

2-bromo-3′,4′-dichloroacetophenone

sodium formate

→

title compound

Ausbeute 42.0%

2-Hydroxy-3′,4′-dichloroacetophenone

Ausbeute 42.0%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturunder reflux
3. 3
   EinengenThe reaction mixture was concentrated
4. 4
   workup.ADDITIONpoured into water (1 L)
5. 5
   FiltrationThe precipitated solid was collected by filtration
6. 6
   Waschenwashed with water
7. 7
   Trocknenwith isopropyl ether, air-dried
8. 8
   Sonstigefurther dried under reduced pressure at 40° C.

Vorschrift

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.

Quelle