HRID844478

反应详情

EQUATION

反应方程式

HRID 844478 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a manner similar to the that of Example B14, a mixture of 3-bromomethyl-3-methyloxetane (468 g, 2.84 mol), 2,2,3,3,4,4,5,5,6,6,7,7,8,8,8-pentadecafluorooctan-1-ol (1032 g, 2.58 mol), tetrabutylammonium bromide (41.5 g), potassium hydroxide (208 g, 3.23 mol), and water (1680 ml) was heated under reflux for 3 hours. GLC analysis revealed complete consumption of starting materials. The reaction mixture was diluted with water, worked-up in the usual manner, and distilled under reduced pressure to give 1,085 g of 15-FOX, representing an overall yield of 87%; bp 82° C./0.1 mm-Hg. The distilled material was >99% pure as indicated by GLC and was used in subsequent polymerization reactions.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 3 hours
  3. customconsumption of starting materials
  4. additionThe reaction mixture was diluted with water
  5. distillationdistilled under reduced pressure
  6. customto give 1,085 g of 15-FOX,
  7. customwas used in subsequent polymerization reactions