HRID250927

反应详情

EQUATION

反应方程式

HRID 250927 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 123.9 mg (0.311 mmol, 1 eq) of methyl 3-[2-amino-3′-(1-methyl-3-pentylureido)biphenyl-4-yl]propanoate in 3 ml of tetrahydrofuran in the presence of 550 μL (0.623 mmol, 2 eq) of 1N lithium hydroxide solution is stirred at room temperature for 4 hours. The reaction medium is concentrated, hydrolyzed with water, acidified with acetic acid and extracted with ethyl acetate. The organic phase is dried over sodium sulfate and evaporated. The residue is taken up in heptane and then recrystallized from acetonitrile. 302.8 mg of 3-[2-amino-3′-(1-methyl-3-pentylureido)biphenyl-4-yl]propanoic acid are obtained in the form of a white powder (m.p.=84.9° C.) Yield=75%

WORKUP

后处理

  1. concentrationThe reaction medium is concentrated, hydrolyzed with water
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. customevaporated
  5. customrecrystallized from acetonitrile