HRID322897

反应详情

EQUATION

反应方程式

HRID 322897 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of ethyl (RS)-4-[2-(4,5-dihydrooxazol-2-yl)-5-(3-thienylmethoxy)phenoxy]-4-(2-methylphenyl)butanoate (500 mg) in methanol (50 mL) containing 10% w/v potassium carbonate (5 mL) is stirred at ambient temperature for 16 hours. The reaction mixture is concentrated under reduced pressure and partitioned between water (100 mL) and ethyl acetate (100 mL) then acidified to pH 5 with 1 N HCl. The organic phase is washed three times with water (50 mL), dried over magnesium sulphate, filtered and concentrated under reduced pressure. Recrystallisation from cyclohexane/ethyl acetate gives (RS)-4-[2-(4,5-dihydrooxazol-2-yl))-5-(3-thienylmethoxy)phenoxy]-4-(2-methylphenyl)butanoic acid hydrate as a white solid (160 mg), m.p. 107-109° C. [Elemental analysis:- C,65.9, H, 5.69, N, 2.94%. Calculated for C25H25NO5S.0.2H2O:- C,66.0, H, 5.59, N, 3.01%].

WORKUP

后处理

  1. concentrationThe reaction mixture is concentrated under reduced pressure
  2. custompartitioned between water (100 mL) and ethyl acetate (100 mL)
  3. washThe organic phase is washed three times with water (50 mL)
  4. dry with materialdried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customRecrystallisation from cyclohexane/ethyl acetate