反应详情

温度

120 °C

A mixture of 4-(7-bromo-3-methyl-3,4-dihydroisoquinolin-2(1H)-yl)-6-chloropyrimidin-2-amine (2.3 g, 6.5 mmol) and 1-methyl piperazine (3.61 mL, 32.6 mmol) in tert-butyl alcohol (10 mL) and was heated at 120° C. for 20 h. The reaction mixture was cooled to r.t., poured into water, extracted with AcOEt, washed with sat'd NaHCO3 aqueous solution and brine, dried with MgSO4. After filtration, the filtrate was concentrated under reduced pressure. The residue was purified by flash chromatography on a silica gel column using 10% methanol in methylene chloride to afford the desired compound. LCMS (M+H)+: m/z=417.1.

1. temperatureThe reaction mixture was cooled to r.t.
2. extractionextracted with AcOEt
3. washwashed with sat'd NaHCO3 aqueous solution and brine
4. dry with materialdried with MgSO4
5. filtrationAfter filtration
6. concentrationthe filtrate was concentrated under reduced pressure
7. customThe residue was purified by flash chromatography on a silica gel column