HRID524225

反应详情

EQUATION

反应方程式

HRID 524225 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.0 g of 5-(3,4-dimethoxyphenyl)-2-{1-[(2-hydroxyphenyl)carbonyl]piperidin-4-yl}-4,4-dimethyl-2,4-dihydro-3H-pyrazol-3-one (compound described in example 94) and 1.0 g potassium carbonate are suspended in 20 ml of acetonitrile. 0.5 g of iodocyclopentane are added and the reaction mixture is heated to reflux for 5 h until the reaction is completed according to TLC analysis. The solvent is evaporated under reduced pressure, and the remaining residue is taken up in EA. The organic phase is washed with water, dried over MgSO4, and the solvent is removed under reduced pressure. Purification of the resulting crude product by crystallization from methanol yields the title compound.

WORKUP

后处理

  1. temperaturethe reaction mixture is heated
  2. temperatureto reflux for 5 h until the reaction
  3. customThe solvent is evaporated under reduced pressure
  4. washThe organic phase is washed with water
  5. dry with materialdried over MgSO4
  6. customthe solvent is removed under reduced pressure
  7. customPurification of the resulting crude product
  8. customby crystallization from methanol