With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.14161-11-6,3,4,5-Trichloropyridazine,as a common compound, the synthetic route is as follows.
PREPARATION 31 3,5-Dichloro-4-(1-methylethylamino)pyridazine A solution of 3,4,5-trichloropyridazine (9.2 g) and isopropylamine (16.5 g) in toluene (25 ml) is refluxed for 18 hr. Excess isopropylamine is removed by atmospheric distillation. The residual solution is cooled and diluted with dichloromethane and aqueous sodium hydroxide solution (5%). The phases are separated. The organic phase is washed with water and then with saline. The organic phase is dried over sodium sulfate and concentrated under reduced pressure to give a liquid which contains a mixture of isomeric products. The isomers are separated by flash chromatography on silica gel eluding with ether/hexane (30/70). The appropriate fractions are pooled and concentrated to give the desired isomer, NMR (CDCl3) 1.33, 4.59, 4.87 and 8.60 delta; CMR (CDCl3) 24.2, 46.4, 117.1, 139.3, 145.5 and 151.3 delta. Further elution gives 3,4-dichloro-5-(1-methylethylamino)pyridazine which is recrystallized from ether hexane, NMR (CDCl3) 1.35, 387, 4.80, and 8.55 delta; CMR (CDCl3) 22.6, 44.7, 116.5, 136.3, 142.5 and 153.4 delta.
The synthetic route of 14161-11-6 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; The Upjohn Company; US5489593; (1996); A;,
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