反応 #2268

反応方程式

chlorotrifluorosuccinic acid

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product

収率 40.7%

2,2,3-trifluorosuccinic Acid

収率 40.7%

溶媒

dioxane

反応条件

後処理

1. 1
   その他to yield a viscous liquid which
2. 2
   その他was decanted from the unreacted zinc
3. 3
   その他Most 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
   抽出The solution was extracted with ether (3×100 ml)
7. 7
   乾燥dried over anhydrous MgSO4

実験手順

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.

出典