HRID34965

反应详情

EQUATION

反应方程式

HRID 34965 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 5 liter, three-neck flask, fitted with a stirrer, reflux condenser, and nitrogen inlet tube, were placed 245 g (2.4 mole) of 3-hydroxymethyl-3-methyloxetane and 3000 ml of p-dioxane. To this solution 47 g (2 mole) of solid sodium metal was added, and the pot temperature was raised to reflux. Heat was maintained until all of the sodium had dissolved. 400 g (2 mole) of 1-bromooctane was added, and the reflux was resumed for 3 days. The mixture was cooled to room temperature, and the solid sodium bromide was filtered off using celite. The solvent was removed by evaporation and the product was distilled at 80° C. and 0.3-mm pressure. Redistillation from calcium hydride gave 231 g of polymerizable monomer, representing a 58 percent yield.

WORKUP

后处理

  1. customInto a 5 liter, three-neck flask, fitted with a stirrer
  2. temperaturereflux condenser, and nitrogen inlet tube
  3. temperaturethe pot temperature was raised
  4. temperatureto reflux
  5. temperatureHeat
  6. dissolutionhad dissolved
  7. filtrationthe solid sodium bromide was filtered off
  8. customThe solvent was removed by evaporation
  9. distillationthe product was distilled at 80° C.
  10. distillationRedistillation from calcium hydride