반응 #422534

반응 방정식

HCl

4-Hydroxy-3,5-dimethoxybenzaldehyde

2-iodoethanol

potassium carbonate

→

4-hydroxyethyloxy-3,5-dimethoxybenzaldehyde

용매

DMF

water

반응 조건

후처리

1. 1
   workup.WAITleft
2. 2
   온도After cooling to RT
3. 3
   추출extracted with chloroform
4. 4
   건조After drying with magnesium sulfate
5. 5
   기타the solvent is removed by distillation
6. 6
   기타the solid is isolated
7. 7
   기타For further purification
8. 8
   기타the solid is purified by column chromatography (flash: ethyl acetate/n-hexane (1:1))

실험 절차

4-Hydroxy-3,5-dimethoxybenzaldehyde (4.99 g, 27.4 mmol), 2-iodoethanol (9.43 g, 54.8 mmol), and potassium carbonate (7.56 g, 27.4 mmol) are added to 50 ml of DMF and left with stirring at 80° C. under a stream of nitrogen for 24 h. After cooling to RT, about 200 ml of water are added to the solution, which is acidified with 10% strength HCl and then extracted with chloroform. After drying with magnesium sulfate, the solvent is removed by distillation and the solid is isolated. For further purification, the solid is purified by column chromatography (flash: ethyl acetate/n-hexane (1:1)).

출처