HRID962404

反应详情

EQUATION

反应方程式

HRID 962404 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2.77 g (0.01 mole) of ethyl 4-cyano-2-diethoxyphosphinyl-2-hydroxybutanoate in 30 ml of CHCl3 is treated with 10.7 g (0.07 mole) of trimethylsilyl bromide. The solution is stirred at 50° for about one day. It's cooled to room temperature, and water is added. The mixture is stirred for about 30 minutes. The layers are separated, and the water layer is washed several times with CHCl3. The water layer is evaporated to dryness under vacuum, and the residue is triturated with acetone to convert it to a solid (filter to collect it), which is 4-cyano-2-hydroxy-2-phosphonobutanoic acid.

WORKUP

后处理

  1. stirringThe mixture is stirred for about 30 minutes
  2. customThe layers are separated
  3. washthe water layer is washed several times with CHCl3
  4. customThe water layer is evaporated to dryness under vacuum
  5. customthe residue is triturated with acetone
  6. filtrationto a solid (filter to collect it), which