Trichloroacetyl isocyanate → (R)-(4-(4-(4-benzoyl-2-methylpiperazin-1-yl)phthalazin-1-yl)phenyl)methyl carbamate

Participants

Reaction Steps

Compound 81 was prepared as described in general Method K. (R)-(4-(4-(4-(hydroxymethyl)phenyl)phthalazin-1-yl)-3-methylpiperazin-1-yl)(phenyl)methanone (JK-28) (125 mg, 0.285 mmol), was dissolved in chloroform (2.50 mL). 2,2,2-trichloroacetyl isocyanate (40.5 μl, 0.342 mmol) was added and the reaction stirred at rt for 80 minutes. The reaction was adsorbed onto alumina (Brockmann II, 3 g), and after 2 hours was eluted with 10% methanol in dichloromethane. The resulting solution was evaporated to give a yellow oil. Chromatography over silica gel with a gradient of hexanes/0-45% ethyl acetate gave a pale yellow solid, compound 81. MS (M+H)+=482.2

Provenance & Evidence