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
A solution of KOH (0.19 g; 3.4 mmol) in ethanol (6 mL) was added to a solution of 2-(Cis-4-tert-butoxycarbonylamino-cyclopent-2-enylmethyl)-malonic acid diethyl ester (1.15 g; 3.2 mmol) in ethanol (6 mL) at 0° C. The reaction mixture was stirred at room temperature overnight, concentrated and ice-water (400 mL) was added. The aqueous phase was washed with diethyl ether (the emulsion formed during the extraction was treated with brine in order to get good phase separation), acidified to pH 3 with 0.5 M HCl, and extracted with diethyl ether. The organic phase was dried and concentrated under reduced pressure to afford 2-(cis4-tert-butoxycarbonylamino-cyclopent-2-enylmethyl)-malonic acid monoethyl ester (0.86 g, 81%) as white crystals.
WORKUP
后处理
- concentrationconcentrated
- additionice-water (400 mL) was added
- washThe aqueous phase was washed with diethyl ether (the emulsion
- customformed during the extraction
- customto get good
- customphase separation),
- extractionextracted with diethyl ether
- customThe organic phase was dried
- concentrationconcentrated under reduced pressure