Dimethyl Sulfate → HCID 178481547, compound

Participants

Reaction Steps

Dimethylsulfate, 1.15g (9mmol), was added to a solution of 1.2g (4.4mmol) of 7-chloro-1,3-dihydro-5-phenyl-2H-pyrazino[2,3-f] [1,4] diazepin-2-one and 1g (9mmol) of potassium t-butoxide in 30 ml of ethanol. After stirring for 10 min at room temperature, the reaction mixture was diluted with 10% aqueous sodium carbonate solution and was extracted with methylene chloride. The extracts were washed with water, dried over sodiumsulfate and evaporated. The residue was chromatographed over 40g of silica gel (Merck, 70-230 mesh) using 10% ethylacetate in methylene chloride. The combined clean fractions were evaporated and the residue was crystallized from ether/hexane to yield the above-named product, with mp. 105°-107°.

Provenance & Evidence