HRID1973121

反应详情

EQUATION

反应方程式

HRID 1973121 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 20 g (0.1 mole) of 2,4,6-trichloroaniline and 12.6 g (0.1 mole) of 1-methyl-3-cyanoguanidine in 10 ml (0.1 mole) of concentrated hydrochloric acid is added 125 ml of n-butanol. The reaction mixture is refluxed for 17 hours, cooled and the alcohol evaporated off. The residue is extracted with ether after making it alkaline with 40% sodium hydroxide. The ether extract is dried over potassium carbonate and evaporated. The residue is dissolved in methanol, the pH adjusted to about 7, charcoal filtered and evaporated. The residue is triturated with ether and the solid that forms is recrystallized from water to obtain 1-(2,4,6-trichlorophenyl)-5-methylbiguanide hydrochloride.

WORKUP

后处理

  1. temperatureThe reaction mixture is refluxed for 17 hours
  2. temperaturecooled
  3. customthe alcohol evaporated off
  4. extractionThe residue is extracted with ether
  5. extractionThe ether extract
  6. dry with materialis dried over potassium carbonate
  7. customevaporated
  8. dissolutionThe residue is dissolved in methanol
  9. filtrationfiltered
  10. customevaporated
  11. customThe residue is triturated with ether
  12. customthe solid that forms is recrystallized from water