HRID232161

反应详情

EQUATION

反应方程式

HRID 232161 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. distillationMost of the trifluoroacetic acid is distilled
  2. customthe final traces are removed under vacuum (12 mm Hg, 50° C.)
  3. filtrationFiltration
  4. washwashing with petroleum