HRID322855

反应详情

EQUATION

反应方程式

HRID 322855 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of methyl (E)-3-(2,4-dibenzyloxyphenyl)-2-cyanoacrylate (400 mg) in tetrahydrofuran (20 mL) containing 0.5 N aqueous lithium hydroxide solution (4 mL) is stirred at ambient temperature for 2 hours. The reaction is concentrated under reduced pressure and the residue taken up in water. This solution is acidified to pH 1 and extracted with diethyl ether. The organic layer is dried over magnesium sulphate, filtered and concentrated under reduced pressure to leave (E)-3-(2,4-dibenzyloxyphenyl)-2-cyanoacrylic acid hydrate as a yellow solid (30 mg). [Elemental analysis:- C, 71.43; H, 5.25; N, 3.47%; Calculated for C24H19NO4.H2O:- C, 71.40; H, 4.81; N, 3.72%].

WORKUP

后处理

  1. concentrationThe reaction is concentrated under reduced pressure
  2. extractionextracted with diethyl ether
  3. dry with materialThe organic layer is dried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure