تفاعل #65121

ord-a5e8b30eff0043a4993d87753dbbf392

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05418224uspto-grants-1995_05