تفاعل #1596

ord-6b35315acbe8476c894bb158bdaa472f

المتفاعلات

الكواشف

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىto yield a viscous liquid which
  2. 2
    أخرىwas decanted from the unreacted zinc
  3. 3
    أخرىMost of the dioxane was evaporated in vacuo
  4. 4
    workup.DISSOLUTIONThe residue was dissolved in 100 ml H2O
  5. 5
    workup.ADDITIONa solution of 7.7 ml of concentrated H2SO4 in 25 ml of water was added
  6. 6
    استخلاصThe solution was extracted with ether (3×100 ml)
  7. 7
    تجفيفdried over anhydrous MgSO4

الإجراء التجريبي

To a stirring solution of the chlorotrifluorosuccinic acid (part b) (24.5 g) in 200 ml dioxane was added portionwise zinc metal (85 g) and the mixture was stirred at ambient temperature for 10 hours to yield a viscous liquid which was decanted from the unreacted zinc. Most of the dioxane was evaporated in vacuo. The residue was dissolved in 100 ml H2O and a solution of 7.7 ml of concentrated H2SO4 in 25 ml of water was added. The solution was extracted with ether (3×100 ml) and dried over anhydrous MgSO4. The organic layer was stripped to yield 8.3 g (32%) of the product as a crystalline solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726162uspto-grants-1998_03