HRID223305

反应详情

EQUATION

反应方程式

HRID 223305 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of ethyl N-trifluoroacetyl-N-(dichlorophosphonomethyl)glycinate (3.3 g, 0.01 mole) in 25 ml. of tetrahydrofuran was added diallylamine (4.07 g, 0.042 mole) in 50 ml. of tetrahydrofuran. The mixture was stirred at room temperature overnight and was then filtered and the filtrate concentrated in vacuo. The residue was dissolved in ether, washed with water, 10% HCl, water, dried over MgSO4, and concentrated in vacuo. The residue was extracted with petroleum ether, and by concentrating the petroleum ether soluble material, ethyl N-trifluoroacetyl-N-(bis(diallylamino)phosphonomethyl)glycinate was obtained as a light yellow oil, ND =1.4536.

WORKUP

后处理

  1. filtrationwas then filtered
  2. concentrationthe filtrate concentrated in vacuo
  3. dissolutionThe residue was dissolved in ether
  4. washwashed with water, 10% HCl, water
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated in vacuo
  7. extractionThe residue was extracted with petroleum ether
  8. concentrationby concentrating the petroleum ether soluble material