1,10-Phenanthroline hydrate → 7-Bromo-2-phenyl-[1,2,4]triazolo[1,5-A]pyridine

関与物質

反応条件

反応手順

A mixture of 2-amino-4-bromopyridine (100.0 g, 0.566 mol), copper (I) bromide (4.15 g, 28.3 mmol), 1,10-phenanthroline monohydrate (5.67 g, 28.3 mmol) and benzonitrile (600 mL) was heated in a 1.5-L autoclave to 130° C. and stirred for 23 h under a continuous gas flow (O2/N2 8:92) of 200 mL/min (constant pressure: 20 bar). After the autoclave was vented and opened (100% conversion, GC method cf. example 1.8), the dark brown reaction suspension was cooled to 0-5° C. and filtered. The filter cake was washed with MeOH (600 mL) and dried to yield crude 7-bromo-2-phenyl-[1,2,4]triazolo[1,5-a]pyridine (120.6 g, 78%) as a green solid with 100% purity (HPLC area-%, GC method cf. example 1.8).

情報源と証拠