Method for synthesizing citric acid ester type compound
A technology of citric acid esters and synthetic methods, which is applied in the preparation of organic compounds, chemical instruments and methods, and preparation of carboxylate esters. It can solve the problems of long process flow, low yield, and many wastes, and shorten the synthetic process. , increase productivity, reduce the effect of three wastes
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Embodiment 1
[0040] Embodiment 1: triethyl citrate is synthesized
[0041] Add 0.2mol (42.0g) of citric acid monohydrate, 0.3g of benzenesulfonic acid, 90ml of 95% (V / V) ethanol and 80ml of water-carrying agent benzene in a three-neck flask with a stirrer and a water separator. Heat to 63-90°C to boil, reflux for 21-49 hours, benzene-ethanol-water forms a ternary minimum azeotrope to distill, cool to normal temperature and the distillate is divided into organic phase and water phase, the organic phase is refluxed, and the water phase is separated out. After the esterification reaction, excess benzene and ethanol were distilled off under reduced pressure. Cool to below 60°C, add 2ml saturated Na 2 CO 3The solution was stirred and neutralized to pH > 8, then transferred to a separatory funnel and allowed to stand for 30 minutes, the brine and the organic phase were separated, and the brine was released, and the organic phase was washed with tap water until neutral. Move the crude product...
Embodiment 2
[0044] Embodiment 2 acetyl triethyl citrate synthesis
[0045] Add 0.2 mol (42.0 g) of citric acid monohydrate, 0.3 g of benzenesulfonic acid, 90 ml of 95% (V / V) ethanol and 80 ml of benzene (water-carrying agent) successively in a three-neck flask equipped with a stirrer and a water separator. Heat to 63-90°C to boil, reflux for 21-49 hours, benzene-ethanol-water forms a ternary minimum azeotrope to distill, cool to normal temperature and the distillate is divided into organic phase and water phase, the organic phase is refluxed, and the water phase is separated out. After the esterification reaction, excess benzene and ethanol were distilled off under reduced pressure. Then add 0.23mol of acetic anhydride, and carry out acetylation reaction at 70°C-90°C for 60-90min; after the acylation reaction is completed, distill off the generated acetic acid and unreacted anhydride under reduced pressure with a jet pump. Cool to below 60°C, add 2ml saturated Na 2 CO 3 The solution w...
Embodiment 3
[0047] Embodiment 3 tributyl citrate is synthesized
[0048] Add 0.2mol (42.0g) of citric acid monohydrate, 0.3g of benzenesulfonic acid and 74g of n-butanol in sequence in a three-necked flask with a stirrer and a water separator, and heat it to a liquid phase of 100-140°C with an oil bath while stirring , reflux reaction for 2.5 hours, n-butanol-water forms a binary minimum azeotrope and distills out. When cooled to normal temperature, the distillate is divided into organic phase and water phase, the organic phase is refluxed, and the water phase is separated. According to the volume of the separated water layer Determine the end point of the reaction. After the esterification reaction was finished, excess butanol was distilled off under reduced pressure. Cool to below 60°C, add 2ml saturated Na 2 CO 3 The solution was stirred and neutralized to pH > 8, then transferred to a separatory funnel and allowed to stand for 30 minutes, the brine and the organic phase were separa...
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