HRID524215

反应详情

EQUATION

反应方程式

HRID 524215 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

0.5 g of 5-(3,4-dimethoxyphenyl)-2-{1-[(5-hydroxy-2-methylphenyl)carbonyl]piperidin-4-yl}-4,4-dimethyl-2,4-dihydro-3H-pyrazol-3-one (compound described in example 85) and 0.3 g potassium carbonate are suspended in 20 ml of DMF. 0.2 ml of ethyl bromoacetate is added and the reaction mixture is heated to 50° C. under a blanket of nitrogen for about 16 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 twice with water and brine, dried over MgSO4, and the solvent is removed under reduced pressure. Purification of the resulting crude product by crystallization from diethyl ether yields the title compound.

WORKUP

后处理

  1. customThe solvent is evaporated under reduced pressure
  2. washThe organic phase is washed twice with water and brine
  3. dry with materialdried over MgSO4
  4. customthe solvent is removed under reduced pressure
  5. customPurification of the resulting crude product
  6. customby crystallization from diethyl ether