N-Methylbenzylamine → HCID 19365588, compound

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Reaction Steps

The compound (1.04 g, 1.8 mmol) obtained in Example 18 was dissolved in dimethylformamide (70 ml). To the solution was added diisopropylaminoethyl(1.15 g, 8.9 mmol) and N-methylbenzylamine (0.54 g, 4.5 mmol) at room temperature, and the mixture was further stirred for one hour. The reaction mixture was concentrated to dryness, and the residue was partitioned between ethyl acetate (300 ml) and water. The aqueous layer was extracted with ethyl acetate (100 ml), the extracts were combined, washed with an aqueous sodium chloride solution, dried with Na2 SO4, and the solvent was distilled off. Thus obtained residue was purified by silica gel column chromatography to give a solid form (1.09 g), and recrystallization from dichloromethane-ether-n-hexane gave pale yellow crystals (1.03 g, 93%).

Provenance & Evidence