HRID1682308

反应详情

EQUATION

反应方程式

HRID 1682308 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.15 g of E-2-formylamino-4-phenyl-5-diethylphosphono-3-pentenoic acid methyl ester are dissolved in 10 ml of 4.5 N hydrochloric acid and heated at 75° for 192 hours. After concentration in vacuo, the foamy residue is dissolved in a small amount of ethanol and 1 ml of ethanol/propylene oxide (1:1) is added dropwise thereto. The resulting white precipitate is filtered off and recrystallised from water/acetone (1:2). E-2-amino-4-phenyl-5-phosphono-3-pentenoic acid is thus obtained in the form of colourless needles, m.p. 230°-233°.

WORKUP

后处理

  1. temperatureheated at 75° for 192 hours
  2. concentrationAfter concentration in vacuo
  3. dissolutionthe foamy residue is dissolved in a small amount of ethanol and 1 ml of ethanol/propylene oxide (1:1)
  4. additionis added dropwise
  5. filtrationThe resulting white precipitate is filtered off
  6. customrecrystallised from water/acetone (1:2)