HRID654660

反应详情

EQUATION

反应方程式

HRID 654660 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a suspension of 3.0 g (9.3 mmol) of diethyl E-2-amino-4-phosphonomethyl-hept-3-ene-1,7-dicarboxylate in 19.1 ml (185.6 mmol) of benzyl alcohol are added 40 ml of a 4N solution of hydrochloric acid in diethyl ether. The solution formed is allowed to stand for 1 week. The reaction mixture is evaporated to dryness. The residue is dissolved in 35 ml of ethanol, and a solution of 35 ml of propylene oxide in 35 ml of ethanol is added. The crystalline precipitate formed is collected, re-crystallized twice from water and dried over phosphorus pentoxide, affording dibenzyl E-2-amino-4-phosphonomethyl-hept-3-ene-1,7-dicarboxylate of m.p. 220°-221° (decomp).

WORKUP

后处理

  1. customThe solution formed
  2. waitto stand for 1 week
  3. customThe reaction mixture is evaporated to dryness
  4. dissolutionThe residue is dissolved in 35 ml of ethanol
  5. additiona solution of 35 ml of propylene oxide in 35 ml of ethanol is added
  6. customThe crystalline precipitate formed
  7. customis collected
  8. customre-crystallized twice from water
  9. dry with materialdried over phosphorus pentoxide