HRID21755

反应详情

EQUATION

反应方程式

HRID 21755 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

The L-proline is dissolved in methanol, the solution is cooled to 0° C. and 36% aqueous formaldehyde is added with stirring. To this solution is then added powdered NaBH4 in portions while maintaining the temperature between -5° and +5° C. The reaction is filtered, the filter cake extracted with solvent and combined with the filtrate, and the solvents evaporated to dryness. The residual N-methyl-L-proline is then dissolved in and reacted with methanol in the presence of H2SO4 at reflux for 4-24 hr. The reaction mixture is cooled to 0° C., and with vigorous stirring a solution of K2CO3 is slowly added to the mixture, until the pH is between pH 7 and 8, then the title product is extracted from the basic mixture and isolated after drying and removal of the solvent.

WORKUP

后处理

  1. additionTo this solution is then added
  2. temperaturewhile maintaining the temperature between -5° and +5° C
  3. filtrationThe reaction is filtered
  4. extractionthe filter cake extracted with solvent
  5. customthe solvents evaporated to dryness
  6. dissolutionThe residual N-methyl-L-proline is then dissolved in and
  7. customreacted with methanol in the presence of H2SO4
  8. temperatureat reflux for 4-24 hr
  9. temperatureThe reaction mixture is cooled to 0° C.
  10. additionis slowly added to the mixture, until the pH
  11. extractionthe title product is extracted from the basic mixture
  12. customisolated
  13. customafter drying
  14. customremoval of the solvent