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2-hydroxy-3,4-dimethoxybromoacetophenone[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With copper(I) bromide; In chloroform; ethyl acetate; at 65℃;
2-Hydroxy-3,4-dimethoxyacetophenone (0.24 g, 1.22 mmol) was added to the reaction flask followed by 6 mL of a mixture of ethyl acetate and chloroform (EA: CHCl3 = 4 mL: 2 mL ), Stirred to dissolve, and then added copper bromide (0.55 g, 2.46 mmol). The mixture was refluxed at 65 C overnight. After the reaction was completed, the mixture was directly filtered with suction and extracted with ethyl acetate (150 mL), washed with saturated brine (100 mL) and dried over anhydrous sodium sulfate. The solvent was removed by rotary evaporation to give the crude product which was used directly in the next reaction.
With potassium carbonate; In acetone; at 62℃; for 6.0h;
2,3,4-trihydroxyacetophenone (1 g, 5.95 mmol) was added to the reaction flask followed by the addition of 20 mL of acetone and the mixture was stirred to dissolve. Then methyl iodide (0.93 mL, 14.94 mmol) and potassium carbonate (3.3 g, 23.88 mmol) and refluxed at 62 C for 6h. The reaction mixture was directly filtered off with suction and extracted with dichloromethane (3 × 50 mL). The organic phases were combined and washed with 3% diluted hydrochloric acid (100 mL), saturated sodium bicarbonate (100 mL) and saturated brine (100 mL) Each wash 1 times, anhydrous sodium sulfate drying. The solvent was removed by rotary evaporation,The crude product was purified by silica gel column chromatography (petroleum ether: ethyl acetate = 2: 1) to give 0.24 g of a white solid,The reaction yield was 21%.
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