HRID745675

反应详情

EQUATION

反应方程式

HRID 745675 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

L-carnitine chloride (1.5. g; 0.008 moles) and 1,4 diazabicyclo[2,2,2]octane (5.25 g; 0.05 moles) were dissolved in 50 cc of DMF at 80° C. The resulting solution was subsequently heated up to 125° C. for 2 hours. Upon reaction termination, the solution was cooled in an ice bath a 5° C. After about 2 hours the precipitate which formed consisting of the excess diazabicyclo octane and its N-methyl derivative was filtered off. DMF was distilled under vacuum and the residue dissolved in water and eluted on AMBERLITE IRA 402 resin activated in the OH-l form. The eluate having alkaline pH was shown to consist of diazabicyclo octane and its N-methyl derivative; L-norcarnitine which formed was retained on the resin and was eluted therefrom with 2N HCl.

WORKUP

后处理

  1. customUpon reaction termination
  2. temperaturethe solution was cooled in an ice bath a 5° C
  3. customAfter about 2 hours the precipitate which formed
  4. filtrationwas filtered off
  5. distillationDMF was distilled under vacuum
  6. dissolutionthe residue dissolved in water
  7. washeluted on AMBERLITE IRA 402 resin