HRID1672724
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
Dissolve cis-4-nitro-benzoic acid 4-(2-oxo-pyrrolidin-1-yl)-cyclohexyl ester (87.9 g, 264 mmol) in methanol (1.35 L) and water (150 mL) and treat with potassium carbonate (109.5 g, 800 mmol). Stir at room temperature overnight to give a white precipitate. Evaporate to dryness. Remove excess water by mixing with ethanol and concentrating to dryness under vacuum. Repeat this procedure. Stir in tetrahydrofuran (1 L) for 1 hour then filter. Evaporate the filtrate to an oil and crystallize from diethyl ether (100 mL) to afford 40 g (83%) of the title compound.
WORKUP
后处理
- customto give a white precipitate
- customEvaporate to dryness
- additionRemove excess water by mixing with ethanol
- concentrationconcentrating to dryness under vacuum
- stirringStir in tetrahydrofuran (1 L) for 1 hour
- filtrationthen filter
- customEvaporate the filtrate to an oil
- customcrystallize from diethyl ether (100 mL)