HRID376147

反应详情

EQUATION

反应方程式

HRID 376147 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.10 g (2.8 mmol) of 5-ethoxy-4-diisopropylphosphonomethyl-2-formylamino-pent-3-enoic acid ethyl ester are dissolved in 20 ml of dichloromethane, and 1.6 ml (12.3 mmol) of trimethylsilane are added dropwise at room temperature. The mixture is left to stand at room temperature for 7 hours, 20 ml of ethanol are added, the mixture is left to stand for a further 15 hours and is concentrated by evaporation, the residue is dissolved in 10 ml of ethanol, and a mixture of 10 ml of propylene oxide and 10 ml of ethanol is added dropwise. A suspension forms, which is stirred at room temperature for 2 hours and is then filtered with suction. Drying yields 5-ethoxy-2-amino-4-phosphonomethyl-pent-3-enoic acid ethyl ester having a melting point of 217°-218° C. (decomp.).

WORKUP

后处理

  1. waitThe mixture is left
  2. waitthe mixture is left
  3. waitto stand for a further 15 hours
  4. concentrationis concentrated by evaporation
  5. dissolutionthe residue is dissolved in 10 ml of ethanol
  6. additiona mixture of 10 ml of propylene oxide and 10 ml of ethanol
  7. additionis added dropwise
  8. filtrationis then filtered with suction
  9. customDrying