Preparation method of high-purity, high-yield β-methylglutaric acid monomethyl ester
A technology of monomethyl methylglutarate and dimethyl methylglutarate, which is applied in the field of organic synthesis, can solve the problems of high raw material prices, low conversion rate of monomethyl ester, and difficult separation, and achieve monoesterification High selectivity, reduced production cost, wide range of raw material sources
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Embodiment 1
[0043] 1. Synthesis of dimethyl β-methylglutarate
[0044] On a 1000ml four-necked reaction flask, install a stirring rod, a thermometer, a dropping funnel and a reflux condenser, add 210g of methanol, slowly add 224g of the crude product of β-methylglutaric acid synthesized in the previous step under stirring, heat to dissolve, add 10g of D001 acid resin that has been activated is heated and refluxed for 2 hours, and the reflux condenser is replaced with a distillation head, a distillation condenser and a water-containing methanol receiver, and 144g of anhydrous methanol is added to the dropping funnel. While adding methanol dropwise, control The reflux temperature does not exceed 80°C, and about 160 g of aqueous methanol is distilled out for about 2 hours.
[0045] The reaction solution was cooled to room temperature, the solid catalyst resin was filtered out, the filter cake was washed with a small amount of methanol, and the filtrates were combined, and the conversion rate...
Embodiment 2
[0054] 1. Synthesis of dimethyl β-methylglutarate
[0055] Install stirring, thermometer, dropping funnel and reflux condenser on a 1000ml four-necked reaction flask, add 240g of methanol, slowly add 224g of synthetic crude β-methylglutaric acid under stirring, heat to dissolve, add 10g of activated D001 acid resin, after heating to reflux for 4 hours, replace the reflux condenser with a distillation head, a distillation condenser and a water-containing methanol receiver, add 240g of anhydrous methanol to the dropping funnel, and control the reflux temperature not to exceed At 80°C, about 350g of aqueous methanol was distilled out for about 4 hours.
[0056] The reaction solution was cooled to room temperature, the solid catalyst resin was filtered out, the filter cake was washed with a small amount of methanol, and the filtrates were combined, and the conversion rate of dimethyl β-methylglutarate reached more than 98.5% according to gas chromatography analysis.
[0057] 2. S...
Embodiment 3
[0065] 1. Synthesis of dimethyl β-methylglutarate
[0066] On a 1000ml four-necked reaction flask, install stirring, thermometer, dropping funnel and reflux condenser, add 320g of methanol, 292g of synthetic crude β-methylglutaric acid, add slowly under stirring, heat to dissolve, add 10g dropwise After the D001 acid resin that has been activated is heated and refluxed for 4 hours, the reflux condenser is replaced with a distillation head, a distillation condenser and a water-containing methanol receiver, and 96g of anhydrous methanol is added to the dropping funnel, and the reflux is controlled while adding methanol dropwise. The temperature does not exceed 80°C, and about 120g of aqueous methanol is distilled out for about 2 hours.
[0067] The reaction solution was cooled to room temperature, the solid catalyst resin was filtered out, the filter cake was washed with a small amount of methanol, and the filtrates were combined, and the conversion rate of dimethyl β-methylglut...
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