反应详情

温度

90 °C

A mixture of 3-[4-(2-chloroethyl)-1-piperidinyl]-6-methylpyridazine (76 mg, 318 μmol), 7-hydroxy-4-ethoxyquinazoline (100 mg, 526 mmol), potassium carbonate (109 mg, 789 mmol) and potassium iodide (53 mg, 319 mmol) in DMF (5 mL) was heated at 90° C. overnight in an argon atmosphere. The mixture was concentrated, and the residue partitioned between ethyl acetate (100 mL), and water (20 mL). The organic phase was dried (MgSO4), filtered, concentrated and purified by column chromatography (silica), using gradient elution (ethyl acetate-methanol/EA). The combined fractions gave a white solid (22 mg, 18%). The 1H nmr data are recorded in Table 6 below.

1. concentrationThe mixture was concentrated
2. customthe residue partitioned between ethyl acetate (100 mL), and water (20 mL)
3. dry with materialThe organic phase was dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated
6. custompurified by column chromatography (silica)
7. washelution (ethyl acetate-methanol/EA)