HRID1054913
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 70 °C
PROCEDURE
实验过程
(2-Amino-6-bromopyridin-3-yloxy)acetic acid methyl ester (4.0 g, 15 mmol) was dissolved in MeOH (40 mL). K2CO3 (3.0 g, 22 mmol) was added and the reaction was stirred at 70° C. for 1 hour. Then, the solvent was removed under reduced pressure and the resulting slurry was suspended in dichloromethane (DCM) and washed with H2O and then brine. The organic layer was dried (Na2SO4) and the product was precipitated from DCM/Et2O to give 6-bromo-4H-pyrido[3,2-b][1,4]oxazin-3-one. Yield 1.9 g (8.3 mmol, 55%). LCMS (ESI): calc. C7H5BrN2O2=228, 230; obs. M+H=229, 231.
WORKUP
后处理
- customThen, the solvent was removed under reduced pressure
- washwashed with H2O
- dry with materialThe organic layer was dried (Na2SO4)
- customthe product was precipitated from DCM/Et2O