HRID275886

反应详情

EQUATION

反应方程式

HRID 275886 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 3-{(3,4-dimethoxy-benzyl)-[({[3-methoxy-4-(3-o-tolylureido)phenyl]-acetyl}-N-methylamino)-acetyl]-amino}-propionic acid [17 g, Example 5(a)] in ethanol (170 ml) was treated with sodium hydroxide solution (23.3 ml, 1N). After stirring at ambient temperature for 24 hours the reaction mixture was filtered through a short pad of diatomaceous earth and then evaporated. The residue was triturated with hot ethyl acetate (200 ml) and dried under vacuum. The resultant foam was dissolved in water (200 ml) and freeze dried for 40 hours to yield the title compound as a white solid (15.4 g), m.p. 225° C. (with decomposition). [Elemental analysis:- C,57.8; H,6.05; N,8.2; Na,3.5%. Calculated for C32H37N4NaO8.2H2O:- C,57.8; H,6.2; N,8.4; Na,3.5%].

WORKUP

后处理

  1. filtrationwas filtered through a short pad of diatomaceous earth
  2. customevaporated
  3. customThe residue was triturated with hot ethyl acetate (200 ml)
  4. customdried under vacuum
  5. dissolutionThe resultant foam was dissolved in water (200 ml)
  6. customfreeze dried for 40 hours