반응 #2168

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chlorotrifluorosuccinic acid

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product

수율 40.7%

2,2,3-trifluorosuccinic acid

수율 40.7%

용매

dioxane

반응 조건

후처리

1. 1
   기타to yield a viscous liquid which
2. 2
   기타was decanted from the unreacted zinc
3. 3
   기타Most 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
   추출The solution was extracted with ether (3×100 ml)
7. 7
   건조dried over anhydrous MgSO4

실험 절차

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.

출처