HRID55377

反应详情

EQUATION

反应方程式

HRID 55377 的结构方程式

PROCEDURE

实验过程

A mixture of 2.6 g of (±)-N"-cyano-N-[3-[[(3,4-dihydro-2H-1-benzopyran-2-yl)methyl]amino]propyl]-N'-(1-methylethyl)guanidine in 20 ml of hydrochloric acid 6N was stirred for 2 hours at reflux temperature. The reaction mixture was evaporated and the residue was dissolved in 10 ml of methanol. This solution was filtered and the filtrate was evaporated. The oily residue was dissolved in 10 ml of ethanol. The mixture was filtered and the filtrate was evaporated, yielding 1.32 g (44.4%) of (±)-N-[3-[[(3,4-dihydro-2H-1-benzopyran-2-yl)methyl]amino]propyl]-N'-(1-methylethyl)-guanidine dihydrochloride; mp. 97.5° C. (comp. 150).

WORKUP

后处理

  1. temperatureat reflux temperature
  2. customThe reaction mixture was evaporated
  3. dissolutionthe residue was dissolved in 10 ml of methanol
  4. filtrationThis solution was filtered
  5. customthe filtrate was evaporated
  6. dissolutionThe oily residue was dissolved in 10 ml of ethanol
  7. filtrationThe mixture was filtered
  8. customthe filtrate was evaporated