反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
In a 10 ml flask, 1-{4-[1-(3,5-dibromo-4-methoxy-benzoyl)-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-7-yl]-phenyl}-ethanone (119 mg, 0.22 mmol), lithium bromide (189 mg, 2.2 mmol) and piperazine (28 mg, 0.33 mmol) were dissolved in 3 ml of N,N-dimethyl formamide, and then stirred at 100° C. for 2.5 hours. After completion of the reaction by adding water dropwise, the mixture was adjusted to weak acidic condition (pH=6) with 1N hydrochloric acid. The formed solid was filtered and washed with distilled water. The resulting solid was recrystallized from methanol to obtain the target compound 67, i.e., 1-{4-[1-(3,5-dibromo-4-hydroxy-benzoyl)-2,3-dihydro-1H-pyrido[2,3-b][1,4]oxazin-7-yl]-phenyl}-ethanone (65 mg, 56%).
WORKUP
后处理
- customAfter completion of the reaction
- filtrationThe formed solid was filtered
- washwashed with distilled water
- customThe resulting solid was recrystallized from methanol