反应详情

温度

120 °C

A mixture of tert-butyl 4-(6-chloropyridazin-3-yl)piperazine-1-carboxylate (0.060 g, 0.20 mmol), compound 83 (0.054 g, 0.20 mmol), Xantphos (0.017 g, 0.030 mmol), Pd2(dba)3 (0.014 g, 0.015 mmol), and sodium tert-butoxide (0.029 g, 0.30 mmol) in dioxane was purged with nitrogen gas for 1 minute. The reaction was heated at 120° C. for 6 hours and then cooled to room temperature. The solvent was removed by filtration. The residue was washed with 2×1 ml dioxane. The product was then dissolved in 10 mL methanol/DCM (1:1) and concentrated. The crude material was re-dissolved in 4 mL methanol and purified on a C-18 reversephase column (150×30 mm, 4 micro) using Mass directed preperative HPLC and gradient elution of acetonitrile in water containing 0.1% TFA to give the title compound 162. LCMS-ESI (POS), M/Z, M+1: 532.3

1. customwas purged with nitrogen gas for 1 minute
2. temperaturecooled to room temperature
3. customThe solvent was removed by filtration
4. washThe residue was washed with 2×1 ml dioxane
5. dissolutionThe product was then dissolved in 10 mL methanol/DCM (1:1)
6. concentrationconcentrated
7. dissolutionThe crude material was re-dissolved in 4 mL methanol
8. custompurified on a C-18 reversephase column (150×30 mm, 4 micro)
9. washHPLC and gradient elution of acetonitrile in water containing 0.1% TFA