HRID230619

反应详情

EQUATION

反应方程式

HRID 230619 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of ethyl {4-[3-(trifluoromethyl)-4,5,6,7-tetrahydro-1H-indazol-1-yl]phenyl}acetate (0.92 g, 2.61 mmol), sodium hydroxide (114 mg, 2.85 mmol), in ethanol (10 ml) and water (10 ml) was stirred at reflux for 1 hour. The reaction mix was allowed to cool and the ethanol was removed under reduced pressure and the residue was made acidic with 5N HCl, then extracted into dichloromethane. The organic layer was added to a 5 g pre-packed column and eluted from 0-100% ethyl acetate in petroleum ether to give the title compound as a pale yellow solid (0.42 g, 50%).

WORKUP

后处理

  1. temperatureat reflux for 1 hour
  2. additionThe reaction mix
  3. temperatureto cool
  4. customthe ethanol was removed under reduced pressure
  5. extractionextracted into dichloromethane
  6. additionThe organic layer was added to a 5 g pre-packed column
  7. washeluted from 0-100% ethyl acetate in petroleum ether