반응 #63243

반응 방정식

sodium

3-hydroxymethyl-3-methyloxetane

sodium

1-bromooctane

→

polymerizable monomer

수율 58.0%

3-Octoxymethyl-3-methyloxetane

수율 58.0%

용매

p-dioxane

반응 조건

후처리

1. 1
   기타Into a 5 liter, three-neck flask, fitted with a stirrer
2. 2
   온도reflux condenser, and nitrogen inlet tube
3. 3
   온도the pot temperature was raised
4. 4
   온도to reflux
5. 5
   온도Heat
6. 6
   workup.DISSOLUTIONhad dissolved
7. 7
   여과the solid sodium bromide was filtered off
8. 8
   기타The solvent was removed by evaporation
9. 9
   workup.DISTILLATIONthe product was distilled at 80° C.
10. 10
    workup.DISTILLATIONRedistillation from calcium hydride

실험 절차

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.

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