HRID476907

反应详情

EQUATION

反应方程式

HRID 476907 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 18 g of N-methyl-2-chloroethylamine hydrochloride, 20 g of 3-mercapto-1,2,4-triazolo(4,3-a)pyridine and 40 ml of triethylamine in 150 ml of ethanol is heated under reflux for 2 hours. After evaporation, the residue is taken up in water, 0.1N sodium hydroxide is added and extraction is carried out with chloroform. The chloroform phase is washed with water, dried over sodium sulfate and evaporated to dryness. The residue obtained is dissolved in an ethyl ether/acetone mixture and the solution is acidified by the addition of a solution of ethyl ether saturated with hydrogen chloride gas. The precipitate formed is filtered off, washed with ether and dried to give 12.6 g of 3-[2-(methylamino)ethylmercapto]-1,2,4-triazolo(4,3-a)pyridine hydrochloride in the form of crystals melting at 195°-7° C.

WORKUP

后处理

  1. temperatureunder reflux for 2 hours
  2. customAfter evaporation
  3. addition0.1N sodium hydroxide is added
  4. extractionextraction
  5. washThe chloroform phase is washed with water
  6. dry with materialdried over sodium sulfate
  7. customevaporated to dryness
  8. customThe residue obtained
  9. customThe precipitate formed
  10. filtrationis filtered off
  11. washwashed with ether
  12. customdried