反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationwas filtered through a short pad of diatomaceous earth
- customevaporated
- customThe residue was triturated with hot ethyl acetate (200 ml)
- customdried under vacuum
- dissolutionThe resultant foam was dissolved in water (200 ml)
- customfreeze dried for 40 hours