HRID232161
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
2,2-Difluorosuccinic acid (120 g, 0.78 moles) and trifluoroacetic anhydride (540 mL) are refluxed (bath temperature 80° C.) for 2 hours. Most of the trifluoroacetic acid is distilled utilizing a short Vigreux column, the final traces are removed under vacuum (12 mm Hg, 50° C.) and finally by stripping twice with carbontetrachloride. The oily residue solidifies on scratching with petroleum ether. Filtration and washing with petroleum either yields 2,2-difluorosuccinic anhydride as slightly violet crystals: 98 g (92%).
WORKUP
后处理
- distillationMost of the trifluoroacetic acid is distilled
- customthe final traces are removed under vacuum (12 mm Hg, 50° C.)
- filtrationFiltration
- washwashing with petroleum