Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 60186-89-2, name is 4-Bromo-2,6-dimethoxypyrimidine. A new synthetic method of this compound is introduced below., Safety of 4-Bromo-2,6-dimethoxypyrimidine
To a solution of 4-bromo-2,6-dimethoxy-pyrimidine (6.80 g, 27.94 mmol) in THF (190 mL) and diethylether (190 mL) n-butyllithium (in hexane/THF, 2.01 g, 30.74 mmol) is added dropwise with stirring at -78 C. After 4 min ethyl trifluoroacetate (4.46 g, 30.74 mmol) in THF (50 mL) is added dropwise at -78 C. The reaction mixture is stirred for 30 min at -78 C and then the reaction is allowed to warm to room temperature slowly and stirred over night at room temperature. To the reaction mixture 1 N HCI solution is added . The resulting mixture is extracted with EA and washed with sat. sodium chloride solution and water. The organic phase is dried over sodium sulfate, filtered and the solvent is evaporated in vacuo. The residue is purified by flash col umn chromatography (silica gel, PE / EA = 8 12) to give the product. MS (ESI+): m/z = 255 [M+H]+ TLC (silica gel, PE/EA 3/1 ): Rf = 0.20
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Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; EICKMEIER, Christian; GERLACH, Kai; HEINE, Niklas; WEBER, Alexander; GROSS, Ulrike; WO2014/127816; (2014); A1;,
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