HRID1075110

反应详情

EQUATION

反应方程式

HRID 1075110 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Cysteamine hydrochloride (3.58 g; 31.5 mmoles) and 6-dimethylaminomethyl-2-hydroxymethylpyridine (5.0 g; 30.1 mmole) [prepared in Step B] were dissolved in 50 ml of 48% hydrobromic acid and the solution heated at reflux temperature for 12 hours and then allowed to stand at ambient temperature for 8 hours. The reaction mixture was evaporated under reduced pressure to half volume, made basic with 40% aqueous NaOH and extracted with several portions of methylene chloride. The combined organic phase was washed with a small amount of water and saturated brine solution then dried and evaporated under reduced pressure to yield 3.14 g of the title compound.

WORKUP

后处理

  1. temperaturethe solution heated
  2. temperatureat reflux temperature for 12 hours
  3. customThe reaction mixture was evaporated under reduced pressure to half volume
  4. extractionextracted with several portions of methylene chloride
  5. washThe combined organic phase was washed with a small amount of water and saturated brine solution
  6. customthen dried
  7. customevaporated under reduced pressure