HRID1810957
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 and 2 mL of 15% aqueous NaOH is added. The mixture is stirred overnight and then concentrated to dryness and suspended in 50 mL of H2O. The pH is adjusted to 4 by careful addition of conc. HCl. The aqueous phase is extracted with 3×100 mL of CH2Cl2. The combined organic phase is dried (MgSO4), filtered and concentrated to give 0.730 g of 2-{4-[2-(3,5-dimethyl-pyrazol-1-yl)-acetyl]-piperazin-1-yl}-benzoic acid in 90% yield.
WORKUP
后处理
- concentrationconcentrated to dryness
- additionThe pH is adjusted to 4 by careful addition of conc. HCl
- extractionThe aqueous phase is extracted with 3×100 mL of CH2Cl2
- dry with materialThe combined organic phase is dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated