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