반응 #1135824

반응 방정식

Acetic acid 3-(4-hydroxy-phenyl)-8-methyl-4-oxo-chroman-7-yl ester

imidazole

→

7-Hydroxy-3-(4-hydroxy-phenyl)-8-methyl-chroman-4-one

용매

EtOH

반응 조건

후처리

1. 1
   온도The reaction mixture was refluxed
2. 2
   기타on a rotary evaporator
3. 3
   workup.ADDITIONpoured
4. 4
   온도chilled
5. 5
   workup.DISTILLATIONdistilled water (1.9 L)
6. 6
   workup.WAITThe water crash out was left
7. 7
   workup.STIRRINGstirring in the cold room overnight
8. 8
   여과The pale pink solid was collected by suction filtration
9. 9
   기타The solid was dried on the freeze dryer for 3 hours (8.31 g, 59%)

실험 절차

Acetic acid 3-(4-hydroxy-phenyl)-8-methyl-4-oxo-chroman-7-yl ester (18.37 g), imidazole (21.18 g, 6 equivalents) and 100% EtOH (536 ml) were added to a round bottom flask (2 L). The reaction mixture was refluxed and monitored by HPLC. The reaction was completed at 8 hours. The reaction mixture was reduced (˜130 ml) on a rotary evaporator and poured into stirred, chilled distilled water (1.9 L). The water crash out was left stirring in the cold room overnight. The pale pink solid was collected by suction filtration. 1H NMR of the solid indicated it was 7-Hydroxy-3-(4-hydroxy-phenyl)-8-methyl-chroman-4-one with >95% purity. The solid was dried on the freeze dryer for 3 hours (8.31 g, 59%).

출처