HRID1943691

反应详情

EQUATION

反应方程式

HRID 1943691 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 10 ml flask, (3,5-dibromo-4-methoxy-phenyl)-[7-(4-trifluoromethyl-phenyl)-2,3-dihydro-pyrido[2,3-b][1,4]oxazin-1-yl]-methanone (122 mg, 0.21 mmol), lithium bromide (148 mg, 1.71 mmol) and piperazine (28 mg, 0.32 mmol) were dissolved in 3 ml of N,N-dimethyl formamide and then stirred at 1000 for 2 hours. After completion of the reaction by adding water dropwise, the mixture was adjusted to weak acidic condition (pH=6) by using 1N hydrochloric acid. The formed solid was filtered and washed with distilled water. The resulting solid was recrystallized from tetrahydrofuran and methanol to obtain the target compound 45, i.e., (3,5-dibromo-4-hydroxy-phenyl)-[7-(4-trifluoromethyl-phenyl)-2,3-dihydro-pyrido[2,3-b][1,4]oxazin-1-yl]-methanone (59 mg, 50%).

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 tetrahydrofuran and methanol