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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
5-bromo-2-bromomethyl-1-phenyl-1H-pyrrole-3-carboxylic acid ethyl ester (400 mg, 0.94 mmol) and tert-butoxycarbonylamino-acetic acid ethyl ester (182 mg, 0.897 mmol) were dissolved in dry N,N-dimethylformamide (7 mL) at 0° C. Sodium hydride (44 mg, 1.08 mmol) was then added in one portion; the mixture was stirred for 30 min at 0° C., quenched by addition of saturated ammonium chloride aqueous solution, and then extracted with ethyl acetate. The organic phase was subsequently washed with saturated sodium chloride aqueous solution, dried with anhydrous sodium sulfate, and filtered, concentrated to give an oil, which was purified by column to give the title compound (392 mg); ESI MS (m/z): 531 (M+Na+).
WORKUP
后处理
- customquenched by addition of saturated ammonium chloride aqueous solution
- extractionextracted with ethyl acetate
- washThe organic phase was subsequently washed with saturated sodium chloride aqueous solution
- dry with materialdried with anhydrous sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customto give an oil, which
- customwas purified by column