Methyl iodide → HCID 23090118, compound

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Reaction Steps

At 0° C., the sodium hydride (washed with pentan and dried, 20.4 mg) was added to a solution of 1-[1-(6-methoxy-3-pyridyl)-5-(2-pyridyl)pyrazole-3-carbonyl]-5-oxo-1,4-diazepane (0.253 g) obtained in Example 108 in N,N-dimethylformamide (5.0 mL), and the mixture was stirred for 15 minutes. To the reaction mixture, methyl iodide (0.0602 mL) was added, and the mixture was stirred at room temperature for 14 hours. The resultant mixture was partitioned between water and chloroform-methanol (5%). The aqueous layer was further extracted with chloroform-methanol (5%), and the organic layers were combined, followed by washing with saturated brine and drying over sodium sulfate anhydrate. After filtration, the solvent was removed under reduced pressure, and the residue was purified through silica gel column chromatography (chloroform-methanol), to thereby give the title compound as an amorphous product (0.231 g, 88%).

Provenance & Evidence