反应详情

In a 5 ml flask, (3,5-dibromo-4-methoxy-phenyl)-(7-methyl-2,3-dihydro-pyrido[2,3-b][1,4]oxazin-1-yl)-methanone (100 mg, 0.23 mmol), lithium bromide (39 mg, 0.45 mmol), piperazine (30 mg, 0.35 mmol) and N,N-dimethyl formamide (1 ml) were added and then stirred at 100□ for 30 minutes. Lithium bromide (39 mg, 0.45 mmol) was further added thereto and then stirred at 1000 for 1 hour. Lithium bromide (39 mg, 0.45 mmol) was further added thereto and then stirred for 1 hour. After neutralizing with saturated solution of sodium hydrogen carbonate to pH 8 to 9, the mixture was adjusted to pH 6 again by using 1N hydrochloric acid. The formed solid was filtered. The resulting solid was purified by column chromatography on silica eluting with a solvent of methanol:dichloromethane=1:30. The fractions containing the product were collected and evaporated to obtain the target compound 27-2 as white solid (74 mg, 76%).

1. stirringstirred at 1000 for 1 hour
2. stirringstirred for 1 hour
3. filtrationThe formed solid was filtered
4. customThe resulting solid was purified by column chromatography on silica eluting with a solvent of methanol
5. additionThe fractions containing the product
6. customwere collected
7. customevaporated