反应详情

温度

130 °C

A mixture of 3-chloro-6-(1-methyl-1H-pyrazol-4-yl)-pyridazine (step d) (4.57 g, 23.6 mmol) and difluoro-quinolin-6-yl-acetic acid hydrazide (step c) (5.60 g, 23.6 mmol) in n-butanol (125 mL) was heated to 130° C. overnight. The mixture was cooled to room temperature, followed by aqueous work up using AcOEt and a solution of K2CO3. The organic layer was dried (MgSO4) and concentrated in vacuo. The residue was purified by flash column chromatography (first chromatography: CH2Cl2 100% and CH2Cl2/MeOH:88/12 followed by another column with toluene/iPrOH/NH4OH:85/15/2) to give the title compound (5.5 g, 62%). M.p=199.7° C.

1. temperatureThe mixture was cooled to room temperature
2. dry with materialThe organic layer was dried (MgSO4)
3. concentrationconcentrated in vacuo
4. customThe residue was purified by flash column chromatography (first chromatography