反应详情

Aluminum (8.06 g, 0.3 mol) and lead bromide (3.7 g, 0.01 mmol) were added to a mixture of 3-hydroxy benzaldehyde (12.3 g, 0.1 mol) was mixed with 200 ml of dimethylformamide. Carbon tetrachloride (61.53 g, 0.4 mol) was slowly added thereto, the mixture was stirred at room temperature for 10 hours, and unreacted solid was filtered to remove therefrom. After sequentially adding 5% HCl, ethylacetate and water thereto, the mixture was extracted three times with ethyl acetate. The combined organic layer was dried over anhydrous magnesium sulfate, filtered and distilled. The resulting residue was subjected to column chromatography (ethyl acetate:n-hexane=1:4) to obtain the title compound (12.57 g, 91%).

1. filtrationunreacted solid was filtered
2. customto remove
3. additionAfter sequentially adding 5% HCl, ethylacetate and water
4. extractionthe mixture was extracted three times with ethyl acetate
5. dry with materialThe combined organic layer was dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. distillationdistilled