Preparation method for 3,5-dimethoxy-2,6-biacyl phenol
A technology of diacylphenol and -diacylphenol, which is applied in the field of preparation of 3,5-dimethoxy-2,6-diacylphenol, can solve the problems of long reaction route, low product purity and complex process, etc. Achieve the effects of less waste, high commercial value, low price and easy availability
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Embodiment 1
[0024] In a 250ml three-necked flask, add 50g of dichloroethane, 16.8g of 1,3,5-trimethoxybenzene, 28g of anhydrous aluminum trichloride, stir and cool down to -10°C; add 15g of acetyl chloride dropwise, and control the reaction temperature- 10~-5°C; heat preservation reaction for 2 hours, then rise to room temperature and stir for 15 hours, slowly pour into 60g of glacial hydrochloric acid with a concentration of 10%, stir, separate liquids, wash the organic phase twice with water and desolvate under reduced pressure to obtain The product is light yellow solid 23g, content 99.1%, melting point 123-124°C, elemental analysis C 12 h 14 o 5 , calculated value (%): C, 60.5; H, 5.92; measured value (%): C, 60.3; H, 6.50; 1 H-NMR (CDCl 3 ,300MHz) δ5.98(s,1H),3.92(s,6H),2.56(s,6H). The yield is 97%.
Embodiment 2
[0026] In a 250ml three-necked flask, add 50g of dichloromethane, 16.8g of 1,3,5-trimethoxybenzene, 53g of anhydrous boron tribromide, stir and cool down to 0°C; add 15g of acetyl chloride dropwise, and control the reaction temperature from 0 to 10°C. ℃; heat preservation reaction for 8 hours, slowly poured into 60g of glacial hydrochloric acid with a concentration of 10%, stirred and separated, and the organic phase was washed twice with water and desolvated under reduced pressure to obtain 22.7g of the product with a content of 98.5% and a yield of 95.5%.
Embodiment 3
[0028] In a 250ml three-necked flask, add 80g of nitrobenzene, 16.8g of 1,3,5-trimethoxybenzene, 28g of anhydrous aluminum trichloride, stir and add 15g of acetyl chloride, the reaction temperature is 60-70°C; keep the temperature for 2 hours, Slowly poured into 60 g of glacial hydrochloric acid with a concentration of 10%, stirred and separated, and the organic phase was washed twice with water and precipitated under reduced pressure to obtain 23.4 g of the product with a content of 98.0% and a yield of 98.6%.
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