HRID2303812

反应详情

EQUATION

反应方程式

HRID 2303812 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. concentrationThe reaction mixture was concentrated and to the residue
  2. additionwas added water
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. customevaporated
  7. customThe residue was purified by chromatography on a silica gel column