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 t-butyl N-{2-[4-(2,4-dioxothiazolidin-5-ylmethyl)phenoxyacetylamino]-5-(4-trifluoromethylphenoxy)phenyl}-N-methylcarbamate (0.95 g) in trifluoroacetic acid (20 ml) was stirred at 60° C. for 3 hours and allowed to stand at ambient temperature overnight. The reaction mixture was concentrated and to the residue was added water and neutralized with aqueous sodium bicarbonate solution (5%). The mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and then evaporated. The residue was purified by chromatography on a silica gel column using n-hexane/ethyl acetate=1/2 as the eluant to give the title compound (0.60 g).
WORKUP
后处理
- concentrationThe reaction mixture was concentrated and to the residue
- additionwas added water
- extractionThe mixture was extracted with ethyl acetate
- washThe ethyl acetate layer was washed with saturated aqueous sodium chloride solution
- dry with materialdried over anhydrous sodium sulfate
- customevaporated
- customThe residue was purified by chromatography on a silica gel column