5-fluoro pyrimidine derivatives
a technology of fluoropyrimidine and derivatives, which is applied in the field of 5fluoropyrimidines and their derivatives, can solve the problems that no single fungicide is useful in all situations, and achieve the effects of convenient use, improved performance and less cos
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Preparation of 5-Fluoro-2-(4-fluorobenzyloxy)pyrimidin-4-amine (1)
[0200]
[0201]To a solution of 4-fluorobenzyl alcohol (2.56 g, 20.3 mmol) in 1,4-dioxane (20 mL) was added 60% NaH (0.813 g, 20.3 mmol) in several portions over a period of 10 min. To the magnetically stirred solution was added 4-amino-2-chloro-5-fluoropyrimidine * (2.00 g, 13.6 mmol) and the mixture was stirred at room temperature until gas evolution subsided. The reaction mixture was then heated in a CEM Discover microwave reactor at 120° C. for 90 min. The cooled reaction mixture was partitioned between ethyl acetate and water, the organic phase was concentrated, and the product was purified by column chromatography (hexane / ethyl acetate gradient) to yield 5-fluoro-2-(4-fluorobenzyloxy)pyrimidin-4-amine (1.66 g, 52% yield) as a white solid: mp 129-131° C.; 1H NMR (300 MHz, CDCl3) δ 7.91 (d, J=2.6 Hz, 1H), 7.42 (m, 2H), 7.03 (m, 2H), 5.27 (s, 2H), 5.05 (br s, 2H); MS (ESI) m / z 238 (M+H)+. *4-Amino-2-chloro-5-fluoropyr...
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