With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.34584-69-5,3,6-Dichloro-4,5-dimethylpyridazine,as a common compound, the synthetic route is as follows.
To a stirred solution of 3,6-dichloro-4,5-dimethylpyridazine (500 mg, 2.82 mmol) in carbon tetrachloride (10 mL) was added nu-bromosuccinimide (503 mg, 2.82 mmol), and AIBnu (2.3 mg, 0.014 mmol) in a round bottom flask equipped with condenser. The reaction was continuously irradiated with a 300 W light and refluxed for 5 h. The formed succimide was filtered and the filtrate was concentrated to afford 4-(bromomethyl)-3,6- dichloro-5-methylpyridazine as a brown solid. To a solution of 4-(bromomethyl)-3,6- dichloro-5-methylpyridazine (400 mg, 1.56 mmol) in DMF was added with benzyl amine (188 muL, 1.72 mmol) and TEA (326 muL, 2.34 mmol). The reaction mixture was heated at 90 0C for 2 h, diluted with DCM and washed with water and brine. The organic layer was dried over Na2SO4 and concentrated to afford a brown oil. The crude material was purified by flash chromatography on silica gel, eluting with 30 – 80percent EtOAc: heptane. Fractions containing the desired product were combined and concentrated to afford a the title compound as a greasy solid (430 mg, yield: 54percent (two steps)). MS (m/z, MH+): meas. 282.2 calc. 282.05, 34584-69-5
The synthetic route of 34584-69-5 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; NOVARTIS AG; WO2008/110611; (2008); A1;,
Pyridazine – Wikipedia
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