Diisopropylethylamine → HCID 59253661, compound

Participants

Reaction Steps

1-chloroethyl chloroformate (2.9 g, 20 mmol) was added dropwise to a stirring mixture of 6-(1-benzyl-piperidin-4-yl)-pyridazin-3-carbonitrile (D2) (1.5 g, 5.1 mmol) and diisopropylethylamine (2.6 g, 20 mmol) in dichloromethane (50 ml) at 0° C. The reaction mixture was stirred at room temperature for 2 h and then the solvent evaporated in vacuo. Methanol (50 ml) was added to the residue and the mixture was refluxed for 2 h. The solvent was evaporated in vacuo and the residue purified by column chromatography (silica gel; 5-12% ammonia in methanol (7M)/dichloromethane). The desired fractions were collected and the solvent evaporated in vacuo to yield D3 (0.9 g, 90%) as a solid. C10H13N5 requires 203. Found 204 (MH+)

Provenance & Evidence