Sodium Bicarbonate → HCID 135760644, compound

Participants

Reaction Steps

In methylene chloride (1000 ml) was dissolved 2-(2-methoxyphenyl)-4-(2-bromophenyl)-4H-1,3,4-oxadiazine-5(6H)-one (91.0 g) obtained in Example 17. Under ice-cooling, 1.0M boron tribromide/methylene chloride solution (900 ml) was added dropwise thereinto over 1 hour, followed by stirring for 1 hour. By adding an aqueous saturated sodium bicarbonate to the reaction solution, the organic layer was separated, and then purified by Cromatorex NH silica gel chromatography (methylene chloride). The resulting crude crystals were recrystallized from methylene chloride/hexane, to give the title compound (62.8 g, 74%).

Provenance & Evidence