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. 4316-97-6, name is 4,6-Dichloro-5-methylpyrimidine. A new synthetic method of this compound is introduced below., Quality Control of 4,6-Dichloro-5-methylpyrimidine
Tert-butyl 4-hydroxypiperidine-1-carboxylate (2.47 g, 12.3 mmol) and potassium tert-butoxide (1.42 g, 12.7 mmol) were added to a THF (20 mL) solution of 2,4-dichloro-3-methylpyrimidine (1.60 g, 9.82 mmol), and the mixture was stirred for 2 hours. To the reaction solution, water was added, followed by extraction with ethyl acetate three times. The obtained organic layer was washed with saturated saline and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=80:20-60:40, V/V) to obtain the title compound as colorless oil (3.07 g, yield: 95%). 1H-NMR (400 MHz, CDCl3) delta ppm: 8.39 (1H, s), 5.36-5.31 (1H, m), 3.75-3.69 (2H, m), 3.75-3.69 (2H, m), 3.39-3.33 (2H, m), 2.23 (3H, s), 2.02-1.95 (2H, m), 1.80-1.72 (2H, m), 1.48 (9H, s).
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Reference:
Patent; Daiichi Sankyo Company, Limited; EP2210886; (2010); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia