HRID1857898
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
C4F9OCH2Cl (50 g, 0.175 mole, isomer ratio n/i=95:5) was combined with sodium iodide (52.5 g, 0.38 mole) in acetone (200 g) and heated to reflux overnight. Water was added and the acetone distilled from the reaction vessel using a Dean-Stark apparatus. The product was washed with water to remove residual acetone. Glc of the residue (52.6 g) revealed it to be 82.6 wt. % of the desired product C4F9OCH2I, which was further purified by distillation. The distillation fraction boiling at 110-115° C. was found to be 97.8 wt. % of the desired product with a 96/4 normal to iso ratio.
WORKUP
后处理
- temperatureheated
- temperatureto reflux overnight
- distillationthe acetone distilled from the reaction vessel
- washThe product was washed with water
- customto remove residual acetone
- distillationwas further purified by distillation