HRID1154287

反应详情

EQUATION

反应方程式

HRID 1154287 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 51 g (0.315 mole) of 2,6-dichloroaniline is added 0.4 moles of ethereal HCl and 200 ml of m-cresol. The mixture is then sitrred and heated on a steam bath to drive off the ether and excess hydrogen chloride. To the resultant mixture is then added 17.7 g (0.315 mole) of methyl cyanamide then heated for 2 hours on a steam bath. The reaction mixture is then cooled, added to 150 ml of conc. sodium hydroxide solution, cooled and extracted with 2 liters of ether. The ether layer is washed with 2×1 liter of water, dried over sodium sulfate, charcoaled and evaporated. The residue is triturated with hexane and the precipitate is filtered off and washed with ether and dried to obtain 1-(2,6-dichlorophenyl)-3-methylguanidine hydrochloride.

WORKUP

后处理

  1. temperatureheated on a steam bath
  2. temperaturethen heated for 2 hours on a steam bath
  3. temperatureThe reaction mixture is then cooled
  4. temperaturecooled
  5. extractionextracted with 2 liters of ether
  6. washThe ether layer is washed with 2×1 liter of water
  7. dry with materialdried over sodium sulfate
  8. customevaporated
  9. customThe residue is triturated with hexane
  10. filtrationthe precipitate is filtered off
  11. washwashed with ether
  12. customdried