HRID412377

反应详情

EQUATION

反应方程式

HRID 412377 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of t-butyl N-[5-(4-t-butoxycarbonylamino-3,5-dimethylphenoxy)-2-[4-(2,4dioxothiazolidin-5-ylmethyl)phenoxyacetylamino]phenyl]-N-methylcarbamate (1.88 g) and 4N hydrogen chloride in 1,4-dioxane (20 ml) was stirred at room temperature for 23 hours. The reaction mixture was concentrated and water added to the residue. The mixture was neutralized with sodium bicarbonate and extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate and concentrated. The residue was chromatographed on a silica gel column using ethyl acetate:n-hexane=2:1 as the eluant to afford the desired compound (0.26 g, mp 209-211° C.).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additionwater added to the residue
  3. extractionextracted with ethyl acetate
  4. dry with materialThe extract was dried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customThe residue was chromatographed on a silica gel column