2-Nitrobenzenesulfenyl chloride → HCID 15136149, compound

Participants

Reaction Steps

To a solution of 0.32 g (1 mmol) of 3-ethoxycarbonyl-9-(dimethylcarbamoylthio)-4-oxo-4H-pyrido[1,2-a]pyrimidine (I d'-1) in 10 ml of dry 1,2-dichloroethane are added 0.2 g (1.5 mmol) of 2-nitrophenylsulphenyl chloride (X) and 0.2 g (1.5 mmol) of zinc chloride, and the resultant mixture is stirred for 35 minutes at room temperature. After the mixture is diluted with 1,2-dichloroethane, it is washed with N-HCl, 5% NaHCO3 and saturated brine in order. The organic layer is dried over sodium sulfate and concentrated under reduced pressure. The residue in 0.5 g is recrystallized from ethyl acetate-methylene chloride to give 0.365 g (Yield: 90.9%) of the titled compound (I e-1).

Provenance & Evidence