반응 #65121

반응 방정식

ammonia

erythromycin A

sodium acetate

iodine

→

N-demethylerythromycin A

수율 40.8%

용매

water

methanol water

반응 조건

후처리

1. 1
   기타the reaction mixture was then irradiated with a quartz lamp at room temperature for 20 minutes
2. 2
   기타Subsequently, half the solvent was evaporated
3. 3
   기타the remaining reaction mixture
4. 4
   추출The reaction mixture was extracted three times with 20 ml portions of methyl t-butyl ether
5. 5
   추출The ether extract
6. 6
   기타was separated
7. 7
   기타some of the ether was evaporated
8. 8
   workup.WAITThe reaction product was then left
9. 9
   기타to crystallize out
10. 10
    기타was recrystallized from acetone

실험 절차

5 g of erythromycin A and 4.7 g of sodium acetate (×3 H2O) were dissolved in 200 ml of an 8:2 methanol/water mixture. 1.75 g of iodine were added to the solution, and the reaction mixture was then irradiated with a quartz lamp at room temperature for 20 minutes. Subsequently, half the solvent was evaporated, and the remaining reaction mixture was poured into a mixture of 140 ml of water and 10 ml of ammonia. The reaction mixture was extracted three times with 20 ml portions of methyl t-butyl ether. The ether extract was separated and some of the ether was evaporated. The reaction product was then left to crystallize out and was recrystallized from acetone. 2 g of N-demethylerythromycin A were obtained.

출처