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
A mixture of 29.1 g (0.50 mol) of dry potassium fluoride' 88.3 g (0.50 mol) of 2-chloroethyl trifluoroacetate, 150 mL of dimethylsulfoxide, and 50 g (0.50 mol) of tetrafluoroethylene was shaken in a 400-mL metal tube at 75° for 18 h. Volatile products were transferred from the reaction mixture held at 43° (1.2 mm). These volatiles were stirred with 500 mL of 10% aqueous NaOH to remove unreacted ester and a small amount of dimethylsulfoxide, then fractionated to afford 61.6 g (47%) of 2-trifluoromethyl-2-pentafluoroethyl-1,3-dioxolane, b.p. 118°-120° . IR (CCl4) and NMR (CCl4) spectra for the product were consistent with the assigned structure. Anal.: Calcd. for C6H4F8O2 : C, 27.71; H, 1.55; F, 58.44. Found: C, 27.57; H, 1.65; F, 58.40.
WORKUP
后处理
- customheld at 43°
- customto remove unreacted ester