HRID2422634

反应详情

EQUATION

反应方程式

HRID 2422634 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

2-{4-[(1-Cyclobutylpiperidin-4-yl)oxy]phenyl}-8-methoxy-3-methylpyrido[3,4-d]pyrimidin-4(3H)-one (500 mg, 1.19 mmol) was dissolved in dichloromethane (1 ml), and with stirring at 0° C., boron trifluoride (1.0 M in CH2Cl2, 3.9 mL) was added thereto, then gradually heated up to room temperature, and stirred at that temperature for 20 hours. The reaction solution was diluted with ethyl acetate, and with cooling with ice, this was poured into aqueous 1 N sodium hydroxide solution, and extracted with ethyl acetate. The organic layer was washed with saturated saline water, and dried with magnesium sulfate. The solvent was evaporated off, and the residue was purified through silica gel column chromatography (chloroform/methanol=1/0 to 9/1 and its polarity was stepwise increased up to 5/1) to obtain the intended compound (300 mg, 62%) as a pale yellow solid.

WORKUP

后处理

  1. temperaturegradually heated up to room temperature
  2. stirringstirred at that temperature for 20 hours
  3. temperaturewith cooling with ice
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with saturated saline water
  6. dry with materialdried with magnesium sulfate
  7. customThe solvent was evaporated off
  8. customthe residue was purified through silica gel column chromatography (chloroform/methanol=1/0 to 9/1 and its polarity
  9. temperaturewas stepwise increased up to 5/1)