Preparation method of 4, 6-dichloro-5-fluoropyrimidine
A technology of fluoropyrimidine and chlorine flow, which is applied in 4 fields, can solve the problems of complex production process reaction, phosphoric acid-containing wastewater, and low product yield, and achieve significant economic and social benefits, no waste residue, and high product purity.
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Embodiment 1
[0015] A method for preparing 4,6-dichloro-5-fluoropyrimidine, using isopentafluorine as a starting material, immersing in a dichloromethane solvent, slowly adding catalyst sulfonyl chloride, and the addition amount is 4,6-dichloropyrimidine 2% of the mass of 5-fluoropyrimidine was irradiated with ultraviolet light with a wavelength of 220 nm for 12 minutes, and then chlorine gas was introduced, the reaction temperature was 20-25 ° C, the chlorine was stirred for 9 hours, the reaction was kept under reflux for 6 hours, the reflux was completed, and the water was separated. layer, evaporated the toluene, and then distilled to obtain 4,6-dichloro-5-fluoropyrimidine mother liquor. After washing the 4,6-dichloro-5-fluoropyrimidine mother liquor with aqueous hydrochloric acid to remove impurities, the product was precipitated again; the product purity was 99.3 %, the total yield is 96%.
Embodiment 2
[0017] A preparation method of 4,6-dichloro-5-fluoropyrimidine, using isopentafluorine as starting material, immersing in dichloroethane solvent, slowly adding catalyst sulfonyl chloride, and the addition amount is 4,6-dichloroethane 4% of the mass of chloro-5-fluoropyrimidine was irradiated with ultraviolet light with a wavelength of 280 nm for 20 minutes, and chlorine gas was introduced, the reaction temperature was 25 ° C, and the chlorine was stirred for 10 hours, and the reaction was kept under reflux for 22 hours. , evaporated the toluene, and then distilled to get the 4,6-dichloro-5-fluoropyrimidine mother liquor. After washing the 4,6-dichloro-5-fluoropyrimidine mother liquor with aqueous sulfuric acid to remove impurities, the product was precipitated again; the product purity was 99.5% , the total yield is 97%.
Embodiment 3
[0019] A method for preparing 4,6-dichloro-5-fluoropyrimidine, using isopentafluorine as a starting material, immersing it in a chloroform solvent, slowly adding catalyst sulfonyl chloride, and the addition amount is 4,6-dichloro-5 -3% of the mass of fluoropyrimidine, irradiated with ultraviolet light with a wavelength of 260 nm for 17 minutes, passed chlorine gas, the reaction temperature was 23 ° C, passed chlorine and stirred for 9 hours, and kept the reflux reaction for 15 hours. Toluene was removed, and then distilled to obtain 4,6-dichloro-5-fluoropyrimidine mother liquor. The 4,6-dichloro-5-fluoropyrimidine mother liquor was washed with citric acid aqueous solution to remove impurities, and the product was precipitated again; the product purity was 99.8% , the total yield is 97%.
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