반응 #50033

반응 방정식

K2CO3

formaldehyde

L-proline

NaBH4

→

N-Methyl-L-proline Methyl Ester

용매

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONTo this solution is then added
2. 2
   온도while maintaining the temperature between -5° and +5° C
3. 3
   여과The reaction is filtered
4. 4
   추출the filter cake extracted with solvent
5. 5
   기타the solvents evaporated to dryness
6. 6
   workup.DISSOLUTIONThe residual N-methyl-L-proline is then dissolved in and
7. 7
   기타reacted with methanol in the presence of H2SO4
8. 8
   온도at reflux for 4-24 hr
9. 9
   온도The reaction mixture is cooled to 0° C.
10. 10
    workup.ADDITIONis slowly added to the mixture, until the pH
11. 11
    추출the title product is extracted from the basic mixture
12. 12
    기타isolated
13. 13
    기타after drying
14. 14
    기타removal of the solvent

실험 절차

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.

출처