反应详情

温度

180 °C

A mixture of 6-bromo-1-chlorophthalazine (Example 1, 0.1 g, 411 μmol), decahydroisoquinoline (114 mg, 821 μmol), potassium carbonate (57 mg, 411 μmol) and 5 mL acetonitrile was added to a glass microwave reaction vessel. The reaction mixture was stirred and heated in a Smith Synthesizer® microwave reactor (Personal Chemistry, Inc., Upssala, Sweden) at 180° C. for 20 min. The mixture was concentrated under vacuum and purified via flash chromatography (silica gel) eluting with a gradient of 2% 2 M ammonia in MeOH/DCM to 6% 2M ammonia in MeOH/DCM to give 6-bromo-1-(octahydroisoquinolin-2(1H)-yl)phthalazine (0.15g) as a yellow solid. Found MS (ES+): 346, 348(M+H)+.

1. additionwas added to a glass microwave reaction vessel
2. concentrationThe mixture was concentrated under vacuum
3. custompurified via flash chromatography (silica gel)
4. washeluting with a gradient of 2% 2 M ammonia in MeOH/DCM to 6% 2M ammonia in MeOH/DCM