반응 #42749

반응 방정식

7-amino-3-(4-chlorophenyl)-8-hydroxy-2-isopropyl-chromen-4-one

sodium formate

→

title compound

N-[3-(4-Chlorophenyl)-8-hydroxy-2-isopropyl-4-oxo-4H-chromen-7-yl]formamide

용매

formic acid

반응 조건

후처리

1. 1
   온도is heated
2. 2
   온도under reflux for 2 h
3. 3
   세척The resulting aqueous suspension is washed with ethyl acetate (2×100 ml)
4. 4
   세척The combined organic layers are washed with water (3×100 ml) and brine (100 ml)
5. 5
   건조dried (magnesium sulfate)
6. 6
   여과filtered
7. 7
   기타The solvent is removed by evaporation in vacuo
8. 8
   기타to afford a dark brown oil
9. 9
   기타This is purified by flash chromatography (hexane/ethyl acetate=1:1, followed by 100% ethyl acetate)

실험 절차

A stirred mixture of 7-amino-3-(4-chlorophenyl)-8-hydroxy-2-isopropyl-chromen-4-one (1.1 g, 3.35 mmol) and sodium formate (0.23 g, 3.35 mmol) in formic acid (50 ml) is heated under reflux for 2 h. After cooling to room temperature, the reaction mixture is poured into ice/water (300 ml) with stirring. The resulting aqueous suspension is washed with ethyl acetate (2×100 ml). The combined organic layers are washed with water (3×100 ml) and brine (100 ml), dried (magnesium sulfate) and filtered. The solvent is removed by evaporation in vacuo to afford a dark brown oil. This is purified by flash chromatography (hexane/ethyl acetate=1:1, followed by 100% ethyl acetate) to afford the title compound.

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