Diethyl Sulfate → HCID 15754480, compound

Participants

Reaction Steps

2.08 g (7.13 mmol) of 4,5,6,7-tetrahydro-4-oxo-3-(4-chloro-2-nitrophenyl)-1H-indazole are dissolved in 80 ml of 10% aqueous sodium hydroxide solution, insolubles are filtered off, and 1.2 g (7.8 mmol) of diethyl sulfate are then added to the solution. Stirring is subsequently continued for 1.5 hours at room temperature and for 1 hour at 0° C., during which process a precipitate starts to separate out after as early as approx. 10 minutes. When the reaction is complete, the precipitate is filtered off with suction and chromatographed on silica gel using ethyl acetate/dichloromethane (1:2). The fraction of Rf =0.72 contains 0.34 g (15.3% of theory) of the desired product of the formula ##STR7## and of melting point 184° C.

Provenance & Evidence