Method for preparing 4-methyl-5-ethoxazole
A technology of ethoxy oxazole and ethoxy is applied in the direction of educts, organic chemistry, products, etc. It can solve the problems of low product yield and purity, long time, low solubility, etc., and achieves mild process reaction conditions and reaction Improved yield and good process stability
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Embodiment 1
[0027] Add 300ml of toluene, 95.66g of 4-methyl-5-ethoxy-1,3-oxazole-2-carboxylic acid ethyl ester (0.48mol), 300ml of drinking water and 23.2g of sodium hydroxide ( 0.58mol), react at 20°C for 3h, separate the liquids, adjust the pH of the aqueous phase to 1.0 with hydrochloric acid, add 300ml of methyl tert-butyl ether, heat up to 30°C and react until no bubbles emerge. Adjust the pH value to 9 with sodium hydroxide, and separate the liquids. The organic phase was distilled under reduced pressure, and the fraction at 60-80°C was collected. 56.9 g of a colorless transparent oil was obtained, with a yield of 93.2%, a gas phase purity of 99.8%, and a liquid phase purity of 99.5%.
Embodiment 2
[0029] Add 1000ml toluene, 110.25g 4-methyl-5-ethoxy-1,3-oxazole-2-carboxylic acid ethyl ester (0.55mol), drinking water, 1000ml and 66.48g sodium hydroxide ( 1.66mol), react at 40°C for 2h, separate the liquids, adjust the pH of the aqueous phase to 2.5 with hydrochloric acid, add 1000ml of chloroform, heat up to 50°C, and react until no bubbles emerge. Adjust the pH value to 11 with sodium hydroxide, and separate the liquids. The organic phase was distilled under reduced pressure, and the fraction at 60-80°C was collected. 66.70 g of a colorless transparent oil was obtained, with a yield of 94.8%, a gas phase purity of 99.6%, and a liquid phase purity of 99.6%.
Embodiment 3
[0031] Put 700L toluene, 100.0Kg ethyl 4-methyl-5-ethoxy-1,3-oxazole-2-carboxylate (502mol), 700Kg drinking water and 40Kg sodium hydroxide (1000mol) into the 2000L reactor , react at 80°C for 1h, separate the liquids, adjust the pH of the aqueous phase to 2.0 with hydrochloric acid, add 700L of dichloromethane, heat up to 40°C and reflux until no bubbles emerge. Adjust the pH value to 13 with sodium hydroxide, and separate the liquids. The organic phase was distilled under reduced pressure, and the fraction at 60-80°C was collected. 60.19Kg of colorless transparent liquid was obtained, the yield was 94.3%, the gas phase purity was 99.7%, and the liquid phase purity was 99.8%.
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