HRID2096262
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationThe mixture is concentrated to dryness
- additionThe pH of the solution is adjusted to 4 by careful addition of conc. HCl
- extractionThe aqueous phase is extracted with 3×100 mL of CH2Cl2
- dry with materialThe organic phase is dried with MgSO4
- filtrationfiltered
- concentrationconcentrated