Hydrogen Peroxide → HCID 86089939, compound

Participants

Reaction Conditions

Reaction Steps

50 parts of 3,4-dimethoxycarbonyl-9-t-butoxy-3,4-diazatricyclo[4,2,1,02,5 ]non-7-ene, 50 parts of KOH and 250 parts of methanol were refluxed for 7 hours, after which 36 parts of 30 percent strength aqueous H2O2 were added dropwise at 60° C. and stirring was continued for a further hour at 60° C. The mixture was cooled to 20° C., and thereafter the solid product was filtered off under suction and washed with 50 parts of methanol, the combined filtrates were evaporated down in a rotary evaporator at from 20° to 40° C. and under 20 mbar, and the residue was extracted in a soxhlet for 12 hours with 300 parts of petroleum ether. The petroleum ether phase was evaporated down to give 28.5 parts (93 mole %) of 9-t-butoxy-3,4-diazatricyclo[4,2,1,02,5 ]nona-3,7-diene of melting point 78° C. (from naphtha). ##STR14##

Provenance & Evidence