反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionTo this solution is then added
- temperaturewhile maintaining the temperature between -5° and +5° C
- filtrationThe reaction is filtered
- extractionthe filter cake extracted with solvent
- customthe solvents evaporated to dryness
- dissolutionThe residual N-methyl-L-proline is then dissolved in and
- customreacted with methanol in the presence of H2SO4
- temperatureat reflux for 4-24 hr
- temperatureThe reaction mixture is cooled to 0° C.
- additionis slowly added to the mixture, until the pH
- extractionthe title product is extracted from the basic mixture
- customisolated
- customafter drying
- customremoval of the solvent