HRID1943736

反应详情

EQUATION

反应方程式

HRID 1943736 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customAfter completion of the reaction
  2. filtrationThe formed solid was filtered
  3. washwashed with distilled water
  4. customThe resulting solid was recrystallized from methanol