Industrial preparation method for 4-chlorine-5-fluorine-2-methyl pyrimidine
A technology of methylpyrimidine and methyltetrahydrofuran, which is applied in the field of preparation of 4-chloro-5-fluoro-2-methylpyrimidine, can solve the problems of toxicity, tear gas and corrosion, and the large amount of phosphorus oxychloride used as a solvent, etc. , to achieve the effect of reducing the generation of related impurities, facilitating the scale-up of production, and making the process safe and controllable
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Embodiment 1
[0015] 5-Fluoro-2-methylpyrimidin-4(3H)-one Synthesis
[0016] 109 g of ethyl formate and 100 g of ethyl fluoroacetate were dissolved in 300 ml of tetrahydrofuran, and 114 g of potassium tert-butoxide and 600 ml of tetrahydrofuran were added. After the drop was completed, the mixture was stirred overnight at room temperature, and the reaction was completed to obtain the intermediate sodium salt of ethyl 2-fluoro-3-oxopropionate. Add 1200 ml of ethanol, 80 g of sodium ethylate, and 97 g of acetamidine hydrochloride, heat the system to reflux and stir overnight, and the reaction is complete. The reaction solution was concentrated to dryness under reduced pressure, dissolved with a minimum amount of water, extracted with 2-methyltetrahydrofuran, concentrated, added ethyl acetate, stirred at room temperature, filtered to obtain 54 grams of 5-fluoro-2-methylpyrimidine-4( 3H)-ketone.
Embodiment 2
[0018] 5-Fluoro-2-methylpyrimidin-4(3H)-one Synthesis
[0019] 109 g of ethyl formate and 100 g of ethyl fluoroacetate were dissolved in 300 ml of isopropyl ether, and 114 g of potassium tert-butoxide and 600 ml of isopropyl ether were added. After the drop was completed, the mixture was stirred overnight at room temperature, and the reaction was completed to obtain the intermediate sodium salt of ethyl 2-fluoro-3-oxopropionate. Add 1200 ml of methanol, 80 g of sodium ethoxide, and 97 g of acetamidine hydrochloride, heat the system to reflux and stir overnight, and the reaction is complete. The reaction solution was concentrated to dryness under reduced pressure, dissolved with a minimum amount of water, extracted with 2-methyltetrahydrofuran, concentrated, added ethyl acetate, stirred at room temperature, filtered to obtain 40 grams of 5-fluoro-2-methylpyrimidine-4( 3H)-ketone.
Embodiment 3
[0021] 5-Fluoro-2-methylpyrimidin-4(3H)-one Synthesis
[0022] 109 g of ethyl formate and 100 g of ethyl fluoroacetate were dissolved in 300 ml of toluene, and 114 g of potassium tert-butoxide and 600 ml of tetrahydrofuran were added. After the drop was completed, the mixture was stirred overnight at room temperature, and the reaction was completed to obtain the intermediate sodium salt of ethyl 2-fluoro-3-oxopropionate. Add 1200 ml of isopropanol, 80 g of sodium ethoxide, and 97 g of acetamidine hydrochloride, heat the system to reflux and stir overnight, and the reaction is complete. The reaction solution was concentrated to dryness under reduced pressure, dissolved with a minimum amount of water, extracted with 2-methyltetrahydrofuran, concentrated, added ethyl acetate, stirred at room temperature, filtered to obtain 30 grams of 5-fluoro-2-methylpyrimidine-4( 3H)-ketone.
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