In the chemical reaction process,reaction time,type of solvent,can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product.An updated downstream synthesis route of 624-95-3 as follows., 624-95-3
2.24 g (51.3 mmol) of 55 wt% sodium hydride was suspended in 100 ml of tetrahydrofuran. 4.24 g (41.5 mmol) of 3,3-dimethylbutanol was added dropwise to the suspension under ice cooling, and the mixture was stirred at room temperature for 15 minutes. To this was added dropwise 20 ml of a tetrahydrofuran solution of 5.0 g (37.7 mmol) of 2-chloro-5-fluoropyrimidine, followed by stirring at room temperature overnight. A saturated aqueous solution of ammonium chloride was added thereto, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate, and the inorganic matter was removed by filtration. The filtrate was concentrated under reduced pressure. The obtained residue was purified by silica gel column chromatography to obtain 4.40 g (22.2 mmol, yield 59%) of 2- (3,3-dimethylbutoxy) -5-fluoropyrimidine.
The chemical industry reduces the impact on the environment during synthesis 624-95-3, I believe this compound will play a more active role in future production and life.
Reference:
Patent; NIPPON SODA COMPANY LIMITED; ITO, SYUICHI; AMANO, TOMOHIRO; IPPOSHI, JUNJI; KOUBORI, SHINYA; (44 pag.)JP2016/30742; (2016); A;,
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