HRID229019

反应详情

EQUATION

反应方程式

HRID 229019 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

Trifluoroacetic acid (5 ml) and methanesulfonic acid (0.2 ml) were added to 6-benzyloxy-7-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinoline (compound 415) (700 mg), and the mixture was stirred at 100° C. for 2 hr. The reaction solution was cooled to room temperature, and the solvent was then removed by distillation under the reduced pressure. A saturated aqueous sodium hydrogencarbonate solution was added to the residue, and the mixture was extracted with chloroform. The chloroform layer was washed with a saturated aqueous sodium hydrogencarbonate solution and water and was then 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 7-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinolin-6-ol (26 mg, yield 5%).

WORKUP

后处理

  1. temperatureThe reaction solution was cooled to room temperature
  2. customthe solvent was then removed by distillation under the reduced pressure
  3. additionA saturated aqueous sodium hydrogencarbonate solution was added to the residue
  4. extractionthe mixture was extracted with chloroform
  5. washThe chloroform layer was washed with a saturated aqueous sodium hydrogencarbonate solution and water
  6. dry with materialwas then dried over anhydrous magnesium sulfate
  7. customThe solvent was removed by distillation under the reduced pressure
  8. customthe residue was purified by column chromatography