反应详情

温度

155 °C

The above crude diamine 2.59-A was dissolved in a mixture of triethylorthoformate:Acetic anhydride (1:1, 9 mL). The reaction mixture was heated to 155° C. for 1 h, cooled to rt and then evaporated. The residue was dissolved in 2.5M NaOH (20 mL) and heated at 50° C. 45 min. The resulting solution was cooled to rt, neutralized with AcOH, and cooled to 0° C. The precipitate was filtered to give 6-bromo-4-chloro-3-methyl-3H-imidazo[4,5-c]pyridine 2.60.

1. temperaturecooled to rt
2. customevaporated
3. dissolutionThe residue was dissolved in 2.5M NaOH (20 mL)
4. temperatureheated at 50° C
5. custom45 min
6. temperatureThe resulting solution was cooled to rt
7. temperaturecooled to 0° C
8. filtrationThe precipitate was filtered