Sodium hydride → HCID 10459001, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 3,6-dichloro-4-(4-trifluoromethyl-phenyl)pyridazine, (Example 45(d)), (100 mg, 0.3 mmol) and 5-hydroxyisoquinoline (112 mg, 0.7 mmol, Aldrich) in DMF (2.5 mL) was added NaH (32 mg, 0.8 mmol, 60% suspension in mineral oil, Aldrich) and the reaction mixture was heated at 140° C. for 10 min in a microwave synthesizer. The reaction mixture was allowed to cool to room temperature and partitioned between H2O/CH2Cl2. The aqueous layer was extracted with CH2Cl2 and the combined organic layers were concentrated in vacuum. The residue was evaporated onto SiO2 and purified by flash silica gel chromatography with 2M NH3 in MeOH/CH2Cl2 (0:1→1:49) as eluant to give the title compound as an white amorphous solid. Mp: 197–199° C. MS (ESI, pos ion.) m/z: 511 (M+1).

Provenance & Evidence