Dimethyl Sulfate → HCID 54520530, compound

Participants

Reaction Steps

To a round bottomed 25 ml flask fitted with a magnetic stirrer bar and nitrogen inlet was added 1,6-dihydro-l-[2-(3-pyridinylcarbonylamino)ethyl]-6-oxo-3-pyridinecarboxylic acid methyl ester (0.211 g, 0.70 mmol) and dimethylformamide (7.0 ml). At room temperature with stirring, sodium hydride (0.018 g, 0.77 mmol, 98% dry) was added. After 45 minutes, the reaction was quenched with dimethylsulfate (0.073 ml, 0.78 mmol). Stirring was continued for 3.75 hours at which time the mixture was concentrated. The crude product was purified by medium pressure liquid chromotography (silica gel, 3% methanol/dichloromethane) and triturated with ether to give the product, MP: 120°-122° C.

Provenance & Evidence