HRID1178220

反应详情

EQUATION

反应方程式

HRID 1178220 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 2,5,6-triamino-4-ethoxy-pyrimidine (10.54 g, 62.37 mmoles) in ethanol (160 ml) was added glyoxal (40% solution in water, 2.7 ml, 18.6 mmoles). The reaction mixture was refluxed for 4 hours. Some insoluble material was filtered off. The filtrate was concentrated in vacuo and the residue purified by flash chromatography (silica, using a CH3OH/CH2Cl2 mixture (5:95) as the eluent), providing the pure title compound (7.34 g, yield: 62%). The spectral data of the product are identical with the literature data (W. Pfleiderer et al. cited supra).

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for 4 hours
  2. filtrationSome insoluble material was filtered off
  3. concentrationThe filtrate was concentrated in vacuo
  4. customthe residue purified by flash chromatography (silica