Synthesis process of flocculant additive 5-fluoroorotic acid
A synthesis process and additive technology, applied in the direction of organic chemistry and the like, can solve the problems of low preparation efficiency of 5-fluoroorotic acid, complex preparation steps, few preparation methods, etc., and achieve short steps, easily available raw materials, and simple operation. Effect
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[0040] Synthesis of 2-dimethoxy-4-hydroxy-5-fluoro-6-carboxylate methyl pyrimidine:
[0041] 10 mL of toluene, 17 g of solid sodium methoxide, and 60 g of dimethyl oxalate were sequentially added to the dry reaction flask, and 9.2 g of methyl fluoroacetate was added dropwise under full stirring, and the temperature was controlled at 25 °C, and the reaction was stirred for 2 hours.
[0042] After adding 4 g of 28% liquid sodium methoxide and 40 g of liquid O-methylisourea sulfate at 35° C. for 8 hours, the solvent was recovered under reduced pressure until the system became viscous.
[0043] 100 mL of water was added, and after the reactants were completely dissolved, the pH was adjusted to 5-6 with hydrochloric acid, a white solid was precipitated, cooled to room temperature, filtered, washed, and dried to obtain 2-dimethoxy-4-hydroxy-5-fluoro- Methyl 6-carboxylate pyrimidine, 70% yield, 99% purity.
[0044] Synthesis of 5-fluoroorotic acid:
[0045] Add 2 g of 2-dimethoxy-4...
Embodiment 2
[0047] Synthesis of 2-dimethoxy-4-hydroxy-5-fluoro-6-carboxylate ethyl pyrimidine:
[0048] 10 mL of toluene, 17 g of solid sodium methoxide and 72 g of diethyl oxalate were sequentially added to the dry reaction flask, and 10.6 g of ethyl fluoroacetate was added dropwise under full stirring, and the temperature was controlled at 30°C, and the reaction was stirred for 2 hours.
[0049] After adding 4 g of 28% liquid sodium methoxide and 40 g of liquid O-methylisourea sulfate at 35°C for 8 hours, 100 mL of water was added, and the layers were stirred and separated. The toluene layer was washed twice with 20 mL of water, and the aqueous phases were combined. The aqueous phase was adjusted to pH=5~6 with hydrochloric acid, and a white solid was precipitated, cooled to room temperature, filtered, washed, and dried to obtain 2-dimethoxy-4-hydroxy-5-fluoro-6-carboxylic acid ethyl ester pyrimidine, yield 62% with a purity of 98.5%.
[0050] Synthesis of 5-fluoroorotic acid:
[0051...
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