HRID541741
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 2,4,5-trichloropyrimidine (0.371 mL, 3.24 mmol) and methyl 3-amino-5-(2-{3-[(tert-butoxycarbonyl)amino]phenyl}ethyl)benzoate (1.20 g, 3.24 mmol) in DMF (20 mL) and potassium carbonate (895 mg, 6.48 mmol) were stirred at 60° C. overnight. The reaction mixture was diluted with 1 N HCl and extracted with ethyl acetate three times. The combined organic solutions were dried with sodium sulfate, filtered, and concentrated in vacuo. The crude residue was purified by flash column chromatography to yield the desired product (1.20 g, 72%). LCMS for C25H26Cl2N4O4Na (M+Na)+: m/z=539.3, 541.3.
WORKUP
后处理
- extractionextracted with ethyl acetate three times
- dry with materialThe combined organic solutions were dried with sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
- customThe crude residue was purified by flash column chromatography