Methanol → 2-[(4-Fluorophenyl)methyl]-7,8-dihydro-10-hydroxy-8-methylpyrazino[1′,2′:1,5]pyrrolo[2,3-d]pyridazine-1,9(2H,6H)-dione

Participants

Reaction Conditions

Reaction Steps

A mixture of 4-bromo-2-(4-fluorobenzyl)-5-(4-methyl-3-oxopiperazin-1-yl)pyridazin-3(2H)-one (0.2 g, 0.51 mmol), dicyclohexylmethylamine (0.15 g, 0.76 mmol), and bis-(tri-t-butylphosphine)palladium (0) (52 mg, 0.10 mmol) in anhydrous methanol (5 mL) was heated in a stainless steel pressure vessel under an atmosphere of carbon monoxide (250 psi) in an oil bath at 90° C. overnight. The resultant mixture was diluted with methanol, filtered through a pad of Celite. The filtrate was concentrated under vacuum. The residual oil was triturated with methanol. The white solid precipitated was filtered to provide the titled dione.

Provenance & Evidence