HRID354869

反应详情

EQUATION

反应方程式

HRID 354869 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A suspension of diethyl [(6-nitro-4-quinazolinylamino)methylene]propanedioate (2.8 g) in N,N-dimethylformamide (152 ml) was shaken with 10% palladium on carbon (0.93 g) in hydrogen atmosphere at ambient temperature for an hour. After the reaction was completed, the catalyst was removed by filtration and washed with chloroform. The combined filtrate and washing was concentrated under reduced pressure to give a residue, to which was added toluene and concentrated under reduced pressure. This operation was repeated to give crystalline diethyl [(6-amino-4-quinazolinylamino)methylene]propanedioate (2.50 g).

WORKUP

后处理

  1. customthe catalyst was removed by filtration
  2. washwashed with chloroform
  3. washThe combined filtrate and washing
  4. concentrationwas concentrated under reduced pressure
  5. customto give a residue
  6. concentrationconcentrated under reduced pressure