Nitrogen → HCID 20515453, compound

Participants

Reaction Conditions

Reaction Steps

0.33 g (0.011 mole) of 80% sodium hydride (in paraffin) are added to a cold solution (5° C.) of 2.3 g (0.01 mole) of 1,2-dimethyl-1,4,9,10-tetrahydropyrrolo[3,2-b][1,5]benzodiazepin-10-one in 20 ml of dry dimethylsulfoxide and 20 ml of tetrahydrofuran under an inert gas atmosphere (N2). The mixture is stirred for 30 minutes and is allowed to come to room temperature (30 minutes). Thereafter, it is again cooled to 5° C. and 1.4 g (0.01 mole) of methyl iodide, dissolved in 5 ml of dry tetrahydrofuran, are added dropwise. After the mixture has been stirred at 35° C. for 2 hours, 50 ml of ice-water are added, and the mixture is extracted several times with ethyl acetate. The combined extracts are concentrated in vacuo, and the residue is chromatographed on neutral silica gel (methylene chloride/methanol), yield: 1.7 g.

Provenance & Evidence