HRID1032697

反应详情

EQUATION

反应方程式

HRID 1032697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.0 g (73.5 mmoles) of 2-hydroxymethylenebutyrolactone sodium salt [synthesized by the method described in J. O. Fissekis et al., J. Org., Chem. 29, 2670 (1964)] and 19.6 g (73.3 mmoles) of 1-amidino-4-benzylpiperazine sulfate were added to 360 ml of ethanol, and the solution was refluxed for 5 hours. Ethanol was evaporated, and the residue was mixed with water and extracted with chloroform. The chloroform layer was dried, concentrated, and purified by silica gel column chromatography to give 6.66 g (yield 29%) of 2-(4-benzylpiperazino)-4-hydroxy-5-(2-hydroxyethyl)pyrimidine as crystals.

WORKUP

后处理

  1. temperaturethe solution was refluxed for 5 hours
  2. customEthanol was evaporated
  3. additionthe residue was mixed with water
  4. extractionextracted with chloroform
  5. dry with materialThe chloroform layer was dried
  6. concentrationconcentrated
  7. custompurified by silica gel column chromatography