19064-64-3, 3,6-Dichloro-4-methylpyridazine is a pyridazine compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated
In a 20 ml microwave flask 3,6-dichloro-4-methylpyridazine (2.30 g, 14.11 mmol) and a 7 M solution OfNH3 in methanol (10.08 ml, 70.6 mmol) were added and heated at 140 C for 4 h under microwave irradiation. After this time the dark brown solution was evaporated and columned on silica gel (flash master, DCM/MeOH form 100/0 to 80/20). Collected fractions gave (0.91 g, 6.33 mmol, 45%) of a 2/1 mixture of 6-chloro-5-methyl-3- pyridazinamine and 6-chloro-4-methyl-3-pyridazinamine. This material was recrystallized from EtOAc: from the first run 6-chloro-4-methyl-3-pyridazinamine (D4) (0.136 g, 0.95 mmol) was obtained. HPLC (walk-up): rt = 1.21 min. MS: (ES/+) m/z: 287 [dimer+1, 100%] and 289 [dimer+1, 66%]. C5H6ClN3 requires 144. UPLC: rt = 0.33, peak observed: 144 (M+ 1, 100%) and 146 (M+l, 33%). 1H NMR (400 MHz, DMSO-J6) delta ppm: 6.74 (s, 1 H) 6.47 (s, 2 H) 2.18 (s, 3 H). The mother liquors were taken and recrystallized with EtOAc other 3 times to give 6-chloro-5-methyl-3-pyridazinamine (0.136 g, 0.95 mmol). HPLC (walk-up): rt = 0.74 min. MS: (ES/+) m/z: 166 [M+Na, 100%] and 168 [M+Na, 33%]. C5H6ClN3 requires 144. UPLC: rt = 0.32, peak observed: 144 (M+l, 100%) and 146 (M+l, 33%). 1H NMR (400 MHz, DMSO-J6) delta ppm: 7.30 (s, 1 H) 6.44 (s, 2 H) 2.08 (s, 3 H).
19064-64-3, The synthetic route of 19064-64-3 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; GLAXO GROUP LIMITED; ALVARO, Giuseppe; AMANTINI, David; BELVEDERE, Sandro; WO2010/60472; (2010); A1;,
Pyridazine – Wikipedia
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