A kind of preparation method of 3-fluoropyruvate
A technology of fluoropyruvic acid and ethyl acetate, which is applied in the field of preparation of 3-fluoropyruvic acid, can solve the problems of low yield, high production cost, long reaction steps and the like, and achieves simple process conditions and low production cost. , the effect of easy operation
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Embodiment 1
[0025] Add 600ml tetrahydrofuran, NaH solid (24.0g, 1.00mol) and diethyl oxalate (140.0g, 0.95mol) into a 1L four-necked round bottom flask equipped with mechanical stirring, slowly Ethyl fluoroacetate (100.0 g, 0.94 mol) was slowly added dropwise, and the reaction was carried out at 70° C. for 6 h after the addition was completed. Add 400ml of toluene, 500.0g of ice, and 88ml of concentrated hydrochloric acid (mass concentration 36-38%) into a 2L beaker, cool down to 0°C, and slowly add the reaction solution dropwise to the 2L beaker to quench excess NaH. Separation, the aqueous layer was extracted with toluene (100ml x 3), the organic phases were combined, after reclaiming the toluene solvent, rectification, and the gas phase temperature of 100-101 ° C was collected to obtain diethyl 2-fluoro-3-oxosuccinate ( 168.9g, 0.82mol), the gas chromatography detection purity is 99.9%, and the yield is 86.9%.
[0026] Gas chromatography testing conditions: Chromatographic column: cap...
Embodiment 2
[0030] Add 1000ml tetrahydrofuran, sodium methoxide solid (80.0g, 2.00mol), diethyl oxalate (280.0g, 1.9mol) in a 2L four-necked round bottom flask equipped with mechanical stirring, and use a constant pressure dropping funnel at room temperature Ethyl fluoroacetate (200.0 g, 1.88 mol) was slowly added dropwise, and the reaction was carried out at 65° C. for 6 h after the addition was completed. Add 400ml of toluene, 1000.0g of ice, and 180ml of concentrated hydrochloric acid (mass concentration 36-38%) into a 5L beaker. Excess sodium hydride. Separation, the aqueous layer was extracted with toluene (100ml x 3), the organic phases were combined, after reclaiming the toluene solvent, rectification, and the gas phase temperature of 100-101 ° C was collected to obtain diethyl 2-fluoro-3-oxosuccinate ( 323.4g (1.57mol), gas chromatography detection purity: 99.9%, yield: 83.5%.
[0031] Add diethyl 2-fluoro-3-oxosuccinate (323.4 g, 1.57 mol) and 200 ml of concentrated hydrochlori...
Embodiment 3
[0033] Add 1000ml tetrahydrofuran, sodium ethoxide solid (136.0g, 2.00mol) and diethyl oxalate (328.0g, 2.28mol) in a 2L four-neck round-bottomed flask equipped with mechanical stirring. Ethyl fluoroacetate (200.0 g, 1.88 mol) was slowly added dropwise, and the reaction was carried out at 60° C. for 6 h after the addition was completed. Add 400ml of toluene, 1000.0g of ice, and 180ml of concentrated hydrochloric acid (mass concentration 36-38%) into a 5L beaker. Excess sodium ethoxide. Separation, the aqueous layer was extracted with toluene (100ml x 3), the organic phases were combined, after reclaiming the toluene solvent, rectification, and the gas phase temperature of 100-101 ° C was collected to obtain diethyl 2-fluoro-3-oxosuccinate ( 327.6g (1.59mol), the gas chromatography detection purity is 99.9%, and the yield is 84.6%.
[0034] Add diethyl 2-fluoro-3-oxosuccinate (327.6g, 1.59mol) into a 1L four-neck flask equipped with mechanical stirring, 200ml of concentrated ...
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