反应详情

温度

90 °C

A mixture of 2-amino-4,6-dichloropyrimidine (0.149 g, 0.908 mmol), 7-bromo-6-fluoro-1,2,3,4-tetrahydroisoquinoline hydrochloride (0.242 g, 0.908 mmol) and, 1,4-dimethylpiperazine (487 uL, 3.63 mmol) in tert-butyl alcohol (2.00 mL, 20.9 mmol) was heated at 90° C. for 2 h. After cooling, 1-methylpiperazine (202 uL, 1.82 mmol) was added. The mixture was heated at 120° C. overnight. After cooling, the volatiles were removed under reduced pressure. The residue was purified by flash chromatography on a silica gel column with methanol in DCM (0-10%) to give the desired product (215 mg, 56.2%). LCMS (M+H)+: m/z=421.1/423.1.

1. temperatureAfter cooling
2. temperatureThe mixture was heated at 120° C. overnight
3. temperatureAfter cooling
4. customthe volatiles were removed under reduced pressure
5. customThe residue was purified by flash chromatography on a silica gel column with methanol in DCM (0-10%)