反应详情

温度

85 °C

To a solution of 640 mg 2-(6-Bromo-3-nitro-pyridin-2-yloxy)-2-methyl-propionic acid methyl ester and 542 mg tin powder were added dropwise 10 ml concentrated hydrochlorid acid upon cooling in an ice bath so that the reaction temperature did not exceed 40° C. The ice bath was then removed and the reaction mixture stirred at 85° C. for one hour. To the cooled reaction mixture was added 100 ml water. The precipitate was collected and dissolved in 300 ml ethyl acetate dried over MgSO4 then the ethyl acetate was removed in vacuo to obtain 335 mg 6-Bromo-3,3-dimethyl-1H-pyrido[2,3-b][1,4]oxazin-2-one as a white solid.

1. temperatureupon cooling in an ice bath so that the reaction temperature
2. customdid not exceed 40° C
3. customThe ice bath was then removed
4. customTo the cooled reaction mixture
5. customThe precipitate was collected
6. dissolutiondissolved in 300 ml ethyl acetate
7. dry with materialdried over MgSO4
8. customthe ethyl acetate was removed in vacuo