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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[0040] Example 1: Synthesis of Triethyl Citrate
[0041] In a three-necked flask with a stirrer and a water separator, 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 with water were added sequentially. Heat to 63~90℃ to boil, reflux for 21~49 hours, benzene-ethanol-water forms the lowest azeotrope of ternary distillate. When cooled to room temperature, the distillate is divided into organic phase and water phase, organic phase is refluxed, and water phase is separated Out. After the esterification reaction, the excess benzene and ethanol are evaporated under reduced pressure. Cool to below 60℃, 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 was separated from the organic phase, the brine was released, and the organic phase was washed with tap water to neutrality. The crude product after...
Example Embodiment
[0044] Example 2 Synthesis of acetyl triethyl citrate
[0045] In a three-necked flask with a stirrer and a water separator, 0.2 mol (42.0 g) of citric acid monohydrate, 0.3 g of benzene sulfonic acid, 90 ml of 95% (V / V) ethanol and 80 ml of benzene (with water agent) were sequentially added. Heat to 63~90℃ to boil, reflux for 21~49 hours, benzene-ethanol-water forms the lowest azeotrope of ternary distillate. When cooled to room temperature, the distillate is divided into organic phase and water phase, organic phase is refluxed, and water phase is separated Out. After the esterification reaction, the excess benzene and ethanol are evaporated under reduced pressure. Then 0.23 mol of acetic anhydride is added, and the acetylation reaction is carried out at 70°C to 90°C for 60 to 90 minutes; after the acylation reaction is completed, the generated acetic acid and unreacted anhydride are evaporated under reduced pressure with a jet pump. Cool to below 60℃, add 2ml saturated Na 2 C...
Example Embodiment
[0047] Example 3 Synthesis of Tributyl Citrate
[0048] Add 0.2mol (42.0g) of citric acid monohydrate, 0.3g of benzenesulfonic acid and 74g of n-butanol to a three-necked flask equipped with a stirrer and a water separator, and heat to liquid phase 100~140℃ with oil bath under stirring. , Reflux for 2.5 hours, the n-butanol-water form binary lowest azeotrope is distilled out. When cooled to room 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 of the reaction. After the esterification reaction, excess butanol was distilled off under reduced pressure. Cool to below 60℃, 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 was separated from the organic phase, the brine was released, and the organic phase was was...
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