HRID322857

反应详情

EQUATION

反应方程式

HRID 322857 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 4-(2,4-dibenzyloxyphenyl)-2,4-dioxobutanoate (2 g) in methanol (100 mL) is treated with 10% aqueous potassium hydroxide (10 mL) and the mixture stirred at room temperature for 18 hours. The reaction mixture is evaporated to low bulk and the residue partitioned between ethyl acetate (100 mL) and 1 N hydrochloric acid (50 mL). The organic phase is washed with water, dried over magnesium sulphate and evaporated in vacuo. The residue iscrystallised from a mixture of ethyl acetate and cyclohexane to give 4-(2,4-dibenzyloxyphenyl)-2,4-dioxobutanoic acid (0.6 g), in the form of a white solid, m.p. 160-164° C. [Elemental analysis:- C,71.3; H,4.93%. Calculated:- C,71.3; H,4.99%].

WORKUP

后处理

  1. customThe reaction mixture is evaporated to low bulk
  2. customthe residue partitioned between ethyl acetate (100 mL) and 1 N hydrochloric acid (50 mL)
  3. washThe organic phase is washed with water
  4. dry with materialdried over magnesium sulphate
  5. customevaporated in vacuo
  6. additionThe residue iscrystallised from a mixture of ethyl acetate and cyclohexane