Preparation method of 3- tertiary butyl-2 and 5- dyhydroxy- benzaldehyde
A technology of tert-butylphenol and tert-butylhydroquinone, applied in the field of preparation of chemical intermediates, can solve the problems of high synthesis cost and complicated process
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Embodiment 1
[0017] 415g of tert-butyl hydroquinone, 1500ml of methanol, nitrogen, heated to reflux, 172g of potassium hydroxide methanol solution was added dropwise, and the temperature was kept for 30min after the addition, and 325g of benzyl chloride was added dropwise, and the dropping time was controlled to be 2 hours. After the dropwise addition, the reaction was refluxed for 6 hours. Methanol was distilled under atmospheric pressure, and after 1200ml was distilled off, 500ml of water and 250ml of ethyl acetate were added for extraction, and 80g of anhydrous sodium sulfate was added for drying. Distill 200ml of the ethyl acetate solution under reduced pressure, add 800ml of a mixture of petroleum ether and ethyl acetate with a volume ratio of 6:2, heat to dissolve, cool to -10°C, and precipitate for 12 hours. Filtration afforded 4-benzyloxy-2-tert-butylphenol.
[0018] 145g of 4-benzyloxy-2-tert-butylphenol, 1500ml of acetic acid, 145g of urotropine, stir and heat up to 80°C, add 46...
Embodiment 2
[0020] 240g of tert-butyl hydroquinone, 800ml of methanol, blow nitrogen, raise the temperature to reflux, dropwise add 80g of potassium hydroxide methanol solution, keep the temperature for 30min after the dropwise addition, add dropwise with 160g of benzyl chloride, and control the dropping time for 2 hours. After the dropwise addition, the reaction was refluxed for 7 hours. Methanol was distilled under atmospheric pressure, and after 700ml was distilled off, 500ml of water and 250ml of ethyl acetate were added for extraction, and 80g of anhydrous sodium sulfate was added for drying. Distill 200ml of the ethyl acetate solution under reduced pressure, add 800ml of a mixture of petroleum ether and ethyl acetate with a volume ratio of 6:2, heat to dissolve, cool to -10°C, and precipitate for 12 hours. Filtration afforded 4-benzyloxy-2-tert-butylphenol.
[0021] 85g of 4-benzyloxy-2-tert-butylphenol, 425ml of acetic acid, 102g of urotropine, stirred and raised to 75°C, added 27...
Embodiment 3
[0023] 780g of tert-butyl hydroquinone, 2000ml of methanol, blow nitrogen, raise the temperature to reflux, dropwise add potassium hydroxide 312g methanol solution, keep warm for 30min after dropping, add dropwise 685g of benzyl chloride, the dropping time is controlled to 2 hours. After the dropwise addition, the reaction was refluxed for 8 hours. Methanol was distilled under atmospheric pressure, and after 1800ml was distilled off, 500ml of water and 250ml of ethyl acetate were added for extraction, and 80g of anhydrous sodium sulfate was added for drying. Distill 200ml of the ethyl acetate solution under reduced pressure, add 800ml of a mixture of petroleum ether and ethyl acetate with a volume ratio of 6:2, heat to dissolve, cool to -10°C, and precipitate for 12 hours. Filtration afforded 4-benzyloxy-2-tert-butylphenol.
[0024] 275g of 4-benzyloxy-2-tert-butylphenol, 1800ml of acetic acid, 412g of urotropine, stirred and heated to 85°C, added 86ml of trifluoroacetic acid...
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