反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
PROCEDURE
实验过程
By the same method as in Example 3, (3,5-dibromo-4-methoxy-phenyl)-(2,3-dihydro-pyrido[3,4-b][1,4]oxazin-1-yl)-methanone (60 mg, 0.140 mmol) and 1M solution of boron tribromide (0.84 ml, 0.840 mmol) were reacted, and then the reaction mixture was neutralized (pH=7) by using saturated solution of sodium hydrogen carbonate and extracted with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate (Na2SO4), filtered and evaporated under reduced pressure to obtain solid. The obtained solid was recrystallized from dichloromethane and n-hexane to obtain the target compound 6, (3,5-dibromo-4-hydroxy-phenyl)-(2,3-dihydro-pyrido[3,4-b][1,4]oxazin-1-yl)-methanone, as white solid (28 mg, 48%).
WORKUP
后处理
- extractionextracted with ethyl acetate
- dry with materialThe combined organic layer was dried over anhydrous sodium sulfate (Na2SO4)
- filtrationfiltered
- customevaporated under reduced pressure
- customto obtain solid
- customThe obtained solid was recrystallized from dichloromethane and n-hexane