反应详情

温度

85 °C

To a solution of 1,2-diamino-4-bromo-pyridinium-2,4,6-trimethyl-benzenesulfonate (Example 1, step a) (8 g, 20.7 mmol) in pyridine (50 ml) was added 3-methoxybenzoyl chloride (6 ml, 41.3 mmol). The reaction mixture was heated at 85° C. for 3 h. Volatiles were removed in vacuum, and the resultant residue was diluted with EtOAc (300 ml). The organic layer was washed successively with water (2×250 ml) and brine (100 ml), dried over anhydrous Na2SO4, filtered, and evaporated in vacuum. The crude material thus obtained was purified by column chromatography over silica gel (10-15% EtOAc/hexane) to afford 7-bromo-2-(3-methoxy-phenyl)-[1,2,4]triazolo[1,5-a]pyridine (8 g, quant) as white solid. LC-MS: m/z=303.8 [M+H]+.

1. customVolatiles were removed in vacuum
2. additionthe resultant residue was diluted with EtOAc (300 ml)
3. washThe organic layer was washed successively with water (2×250 ml) and brine (100 ml)
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. customevaporated in vacuum
7. customThe crude material thus obtained
8. customwas purified by column chromatography over silica gel (10-15% EtOAc/hexane)