Imidazole → HCID 57581529, compound

Participants

Reaction Conditions

Reaction Steps

Compound 77 was prepared as described in general Method I. A 15 mL Schlenk tube was charged with (S)-(4-(4-chlorophthalazin-1-yl)-2-methylpiperazin-1-yl)(phenyl)methanone JK-4 (100 mg, 0.273 mmol), 1H-imidazole (22.3 mg, 0.328 mmol), copper (I) iodide (2.6 mg, 0.0136 mmol), potassium phosphate (122 mg, 0.573 mmol), trans-cyclohexanediamine (3.3 μl, 0.0273 mmol), and dioxane (0.75 mL). The vessel was evacuated, backfilled with argon 5 times, and then heated at 110° C. for 22 hours. After cooling, the reaction was then taken up in ethyl acetate (80 mL) and washed with aqueous K2CO3 (10%), water, and saturated sodium chloride. The organics were dried (MgSO4) and evaporated to give a yellow oil. Chromatography over silica gel with a gradient of hexanes/0-100% ethyl acetate gave a white solid, compound 77. MS (M+H)+=399.2.

Provenance & Evidence