HRID2096262

反应详情

EQUATION

反应方程式

HRID 2096262 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-{4-[2-(3,5-dimethyl-pyrazol-1-yl)-acetyl]-piperazin-1-yl}-benzoic acid methyl ester (0.848 g, 2.38 mmol) is dissolved in 10 mL of 1:1 THF/MeOH. 2 mL of 15% aq NaOH is added and the mixture is stirred overnight. The mixture is concentrated to dryness and suspended in 50 mL of H2O. The pH of the solution is adjusted to 4 by careful addition of conc. HCl. The aqueous phase is extracted with 3×100 mL of CH2Cl2. The organic phase is dried with MgSO4, filtered and concentrated to give 0.730 g of {4-[2-(3,5-dimethyl-pyrazol-1-yl)-acetyl]-piperazin-1-yl}-benzoic acid in 90% yield.

WORKUP

后处理

  1. concentrationThe mixture is concentrated to dryness
  2. additionThe pH of the solution is adjusted to 4 by careful addition of conc. HCl
  3. extractionThe aqueous phase is extracted with 3×100 mL of CH2Cl2
  4. dry with materialThe organic phase is dried with MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated