반응 #76214

반응 방정식

2-bromo-3′,4′-dichloroacetophenone

sodium formate

→

title compound

수율 42.0%

2-Hydroxy-3′,4′-dichloroacetophenone

수율 42.0%

용매

methanol

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux
3. 3
   농축The reaction mixture was concentrated
4. 4
   workup.ADDITIONpoured into water (1 L)
5. 5
   여과The precipitated solid was collected by filtration
6. 6
   세척washed with water
7. 7
   건조with isopropyl ether, air-dried
8. 8
   기타further dried under reduced pressure at 40° C.

실험 절차

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.

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