HRID1530702

反应详情

EQUATION

反应方程式

HRID 1530702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of the above crude 13-(1-ethoxyethenyl)-12-fluoro-4-[3-methyl-1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene (1.97 g, 4.93 mmol) and p-toluenesulfonic acid (90 mg, 0.50 mmol) in acetone (10.0 ml) was heated under reflux for 30 min. Evaporation under reduced pressure gave a yellow solid, which was purified using flash chromatography on silica gel using 4% dichloromethane in methanol as eluant to afford the title compound (1.55 g, 85% yield for two steps). LCMS m/z [M+H]+ 370.1

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 30 min
  3. customEvaporation under reduced pressure
  4. customgave a yellow solid, which
  5. customwas purified