HRID2303834

反应详情

EQUATION

反应方程式

HRID 2303834 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl chloroformate (87 mg) was added dropwise to a solution of cyclohexanecarboxylic acid (90 mg) and triethylamine (232 mg) in anhydrous N,N-dimethylformamide (8 ml) at ambient temperature. The mixture was stirred at the same temperature for 1.5 hours. To the reaction mixture was added 5-{4-[6-(4-aminophenoxy)-1-methyl-1H-benzimidazole-2-ylmethoxy]benzyl}thiazolidine-2,4-dione dihydrochloride (400 mg) in small portions. The mixture was stirred at 50° C. for 1.5 hours. The reaction mixture was concentrated and partitioned between ethyl acetate and water. The ethyl acetate layer was dried over anhydrous sodium sulfate and concentrated. On addition of ethyl acetate to the residue insoluble product was formed and isolated by filtration and washed with ethyl acetate to give the title compound (262 mg).

WORKUP

后处理

  1. stirringThe mixture was stirred at 50° C. for 1.5 hours
  2. concentrationThe reaction mixture was concentrated
  3. custompartitioned between ethyl acetate and water
  4. dry with materialThe ethyl acetate layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. additionOn addition of ethyl acetate to the residue insoluble product
  7. customwas formed
  8. customisolated by filtration
  9. washwashed with ethyl acetate