반응 #11824

반응 방정식

1-(5-chloro-2-hydroxy-phenyl)-ethanone

magnesium methylcarbonate

bromoacetonitrile

→

title compound

수율 58.6%

4-(5-Chloro-2-hydroxy-phenyl)-4-oxo-butyronitrile

수율 58.6%

용매

hydrochloric acid

반응 조건

후처리

1. 1
   온도The reaction was cooled to ambient temperature
2. 2
   추출This was extracted with ethyl acetate
3. 3
   세척washed with brine
4. 4
   건조dried over magnesium sulfate
5. 5
   여과filtered
6. 6
   농축concentrated

실험 절차

A solution of 1-(5-chloro-2-hydroxy-phenyl)-ethanone (1.0 g, 5.86 mmol) and magnesium methylcarbonate (13 mL, 32.5 mmol, 2.5 M solution in DMF) was stirred at 120° C. for 3 hours. The mixture was cooled to ambient temperature followed by the addition of bromoacetonitrile (1.22 mL, 17.6 mmol). The resulting solution was stirred at 90° C. for 3 hours. The reaction was cooled to ambient temperature then slowly poured into 1 M hydrochloric acid (200 mL). This was extracted with ethyl acetate, washed with brine, dried over magnesium sulfate, filtered and concentrated. Flash chromatography on silica gel gave the title compound (0.72 g).

출처