반응 #63242

반응 방정식

3,3-bis(chloromethyl)oxetane

2-methoxyethanol

sodium

sodium

→

required monomer

3,3-Bis(methoxyethoxymethyl)oxetane

반응 조건

후처리

1. 1
   기타To a 5 liter, three-neck flask, fitted with a reflux condenser, a stirrer
2. 2
   온도The flask temperature was then raised
3. 3
   온도to mild reflux
4. 4
   workup.DISSOLUTIONhad dissolved
5. 5
   온도heating
6. 6
   온도maintained for a further 24 hr
7. 7
   기타the precipitated sodium chloride removed by filtration
8. 8
   workup.DISSOLUTIONThe filtrate was dissolved in an excess of water
9. 9
   추출extracted with four portions of 500 ml methylene chloride
10. 10
    건조the combined organic layers were dried over magnesium sulfate
11. 11
    기타The solvent was then removed by evaporation

실험 절차

To a 5 liter, three-neck flask, fitted with a reflux condenser, a stirrer, and a thermometer, were added 1824 g (24 mole) of 2-methoxyethanol followed by 139 g (6 mole) of sodium metal. The flask temperature was then raised to mild reflux and thus maintained until all the sodium had dissolved. At this time, 465 g (3 mole) of 3,3-bis(chloromethyl)oxetane was added and heating maintained for a further 24 hr. The mixture was then cooled to room temperature and the precipitated sodium chloride removed by filtration. The filtrate was dissolved in an excess of water, extracted with four portions of 500 ml methylene chloride, and then the combined organic layers were dried over magnesium sulfate. The solvent was then removed by evaporation and the required monomer isolated by fractional distillation, the fraction boiling at 85° C. and 0.1-mm pressure being collected. Redistillation from calcium hydride yielded 487 g of polymerizable grade monomer.

출처