HRID322867

反应详情

EQUATION

反应方程式

HRID 322867 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

A mixture of methyl (RS)-5-(3-benzyloxy-phenyl)-4-(3-methylpyrid-4-yl)-5-oxopentanoate (3.26 g), dioxan (50 mL), water (9 mL) and concentrated hydrochloric acid (6 mL) is stirred at 60° C. for 1 hour and then evaporated to dryness under reduced pressure. The residue is treated with saturated aqueous sodium bicarbonate solution to give a solution of pH 7 and extracted with ethyl acetate. Evaporation, followed by crystallisation from a mixture of ethyl acetate and pentane affords (RS)-5-(3-benzyloxyphenyl)-4-(3-methylpyrid-4-yl)-5-oxopentanoic acid (1.56 g) in the form of a cream coloured solid, m.p. 55-57° C. [Elemental analysis:- C,73.7;H,5.92; N,3.41%. Calculated:- C,74.0;H,5.95;N,3.60%].

WORKUP

后处理

  1. customevaporated to dryness under reduced pressure
  2. additionThe residue is treated with saturated aqueous sodium bicarbonate solution
  3. customto give a solution of pH 7
  4. extractionextracted with ethyl acetate
  5. customEvaporation
  6. customfollowed by crystallisation from a mixture of ethyl acetate and pentane