HRID2303827

反应详情

EQUATION

反应方程式

HRID 2303827 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 5-{4-[6-(4-aminophenoxy)-1-methyl-1H-benzimidazole-2-ylmethoxy]benzyl}thiazolidine-2,4-dione dihydrochloride (400 mg), acetylchloride (71 mg), triethylamine (263 mg) and anhydrous N,N-dimethylformamide (8 ml) was stirred at ambient temperature for 1 hour. The reaction mixture was concentrated and partioned between ethyl acetate and water. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution and dried over anhydrous sodium sulfate and concentrated. The residue was purified by chromatography on a silica gel column using n-hexane/ethyl acetate=1/4→ethyl acetate→ethyl acetate/methanol=1/10 as the eluant to give the title compound (320 mg).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. washThe ethyl acetate layer was washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated
  5. customThe residue was purified by chromatography on a silica gel column