HRID61908

反应详情

EQUATION

反应方程式

HRID 61908 的结构方程式

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Mixture of 3-(3-hydroxy-pyridin-4-yl)-7-methoxy-1,1-dimethyl-3,4-dihydro-1H-naphthalen-2-one (Compound GT15-9, 270 mg) and methanesulfonic acid (1 ml) was stirred and heated at 110° C. for 0.5 hrs. After cooling, the reaction mixture was neutralized with 2 N aqueous solution of sodium hydroxide. The resulting mixture was extracted with the mixture of DCM and MeOH (DCM:MeOH=9:1). The organic layer was concentrated under reduced pressure, and the resulting residues were purified by silica gel column (DCM/MeOH) to obtain the title compound (110 mg, 43%).

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionThe resulting mixture was extracted with the mixture of DCM and MeOH (DCM:MeOH=9:1)
  3. concentrationThe organic layer was concentrated under reduced pressure
  4. customthe resulting residues were purified by silica gel column (DCM/MeOH)