HRID710068

反应详情

EQUATION

反应方程式

HRID 710068 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

A sealed tube was charged with a mixture prepared by adding toluene (2 ml) to Compound 18 (30 mg), 4-bromopyridazine hydrobromide (22 mg), Pd(OAc)2 (2 mg), Cs2CO3 (37 mg), and [1,1′-binaphthalen]-2-yldi-tert-butylphosphine (3 mg) and the mixture was stirred at 100° C. for 4 hours. After cooling the reaction mixture to room temperature, NH silica gel was added, followed by stirring for a while. After separating the silica gel by filtration, the silica gel was washed with chloroform and the solvent was distilled off; the resulting residue was purified by reverse-phase preparative HPLC to give the titled compound (6.0 mg, colorless oil.)

WORKUP

后处理

  1. additionA sealed tube was charged with a mixture
  2. customprepared
  3. temperatureAfter cooling the reaction mixture to room temperature
  4. additionNH silica gel was added
  5. stirringby stirring for a while
  6. customAfter separating the silica gel
  7. filtrationby filtration
  8. washthe silica gel was washed with chloroform
  9. distillationthe solvent was distilled off
  10. customthe resulting residue was purified by reverse-phase preparative HPLC