HRID228907

反应详情

EQUATION

反应方程式

HRID 228907 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

1-[2-(7-Benzyloxy-6-methoxy-quinolin-4-yloxy)-5-methoxy-phenyl]-ethanone (2.52 g) was suspended in a mixed solution composed of methanesulfonic acid (3 ml) and trifluoroacetic acid (50 ml), and the suspension was stirred at 70° C. for 30 min. The solvent was removed by distillation under the reduced pressure, water was added to the residue, and the mixture was neutralized with sodium hydrogencarbonate powder and was then extracted with chloroform. The chloroform layer was then washed with water and saturated brine and was dried over anhydrous magnesium sulfate, the solvent was removed by distillation under the reduced pressure, and the residue was purified by column chromatography using chloroform-methanol to give the title compound (1.23 g, yield 62%).

WORKUP

后处理

  1. customThe solvent was removed by distillation under the reduced pressure, water
  2. additionwas added to the residue
  3. extractionwas then extracted with chloroform
  4. washThe chloroform layer was then washed with water and saturated brine
  5. dry with materialwas dried over anhydrous magnesium sulfate
  6. customthe solvent was removed by distillation under the reduced pressure
  7. customthe residue was purified by column chromatography