Methylhydrazine → HCID 86724094, Verbindung

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

To the suspension of 1-methyl-3-(pyrimidin-4-yl)-1H-pyrazol-5-amine (0.42 g, 2.4 mmol, prepared using A with methylpyrimidine-4-carboxylate (Ark Pharm) with NaH followed by B with methyl hydrazine) and 4-bromo-2-methylbenzaldehyde (0.48 g, 2.40 mmol, Ark Pharm) in acetonitrile (15 mL) was added p-TSA (0.09 g, 0.5 mmol) and heated to about 50° C. for about 5 h. The reaction mixture was cooled to ambient temperature and continued to stir for about 16 h. The precipitate was collected by filtration and dried under reduced pressure to afford 4-(4-bromo-2-methylbenzylidene)-1-methyl-3-(pyrimidin-4-yl)-1H-pyrazol-5(4H)-imine (0.43 g, 51%) as a light brown solid. LC-MS MS (Table 1, Method g) Rt=2.48 min, m/z 356, 358 (M+H)+.

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