تفاعل #215022

ord-edfcff491d234780b5e2cf47c76295da

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added to the solution
  2. 2
    تركيزThe reaction mixture was concentrated at a low temperature
  3. 3
    workup.DISTILLATIONafter which ethyl acetate and distilled water
  4. 4
    workup.ADDITIONwere added to the residue
  5. 5
    workup.STIRRINGThe resulting mixture was shaken
  6. 6
    أخرىthe aqueous layer was separated
  7. 7
    أخرىThe oily substance thus precipitated
  8. 8
    استخلاصwas extracted with ethyl acetate
  9. 9
    غسيلthe extract was washed with water
  10. 10
    تجفيفdried over anhydrous magnesium sulfate
  11. 11
    أخرىevaporated under reduced pressure
  12. 12
    أخرىto remove the solvent

الإجراء التجريبي

In 150 ml of methanol was dissolved 5.0 g of the above ester, and 20 ml of 1N sodium hydroxide solution was added to the solution. The mixture was stirred at room temperature for 8 hrs. The reaction mixture was concentrated at a low temperature, after which ethyl acetate and distilled water were added to the residue. The resulting mixture was shaken, and the aqueous layer was separated and made weakly acidic with 10% hydrochloric acid solution. The oily substance thus precipitated was extracted with ethyl acetate, and the extract was washed with water and dried over anhydrous magnesium sulfate, and thereafter evaporated under reduced pressure to remove the solvent, thereby obtaining 3.0 g (yield 65%) of a colorless oily substance of N-benzoyl-L-valyl-L-leucine.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04257940uspto-grants-1981_03