HRID534906
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred solution of ethyl 2-[4-(2-tert-butylphenyl)piperazin-1-yl]-2-oxoacetate (0.067 g, 0.21 mmol) in THF (3.0 mL) was added a solution of lithium hydroxide (0.025 g, 1.04 mmol) in water (2.0 mL) at room temperature. After 1 h the reaction mixture was extracted with ethyl acetate (1×5.0 mL) and the aqueous solution acidified with 1 M hydrochloric acid to pH 6. The aqueous layer was extracted with 3:1 chloroform/2-propanol (2×10.0 mL). The combined organics were dried (Na2SO4), filtered, and concentrated under reduced pressure providing 2-[4-(2-tert-butylphenyl)piperazin-1-yl]-2-oxoacetic acid (0.031 g, 51%) as a white solid.
WORKUP
后处理
- extractionAfter 1 h the reaction mixture was extracted with ethyl acetate (1×5.0 mL)
- extractionThe aqueous layer was extracted with 3:1 chloroform/2-propanol (2×10.0 mL)
- dry with materialThe combined organics were dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated under reduced pressure