反応 #63242

反応方程式

3,3-bis(chloromethyl)oxetane

2-methoxyethanol

sodium

sodium

→

required monomer

3,3-Bis(methoxyethoxymethyl)oxetane

反応条件

後処理

1. 1
   その他To a 5 liter, three-neck flask, fitted with a reflux condenser, a stirrer
2. 2
   温度The flask temperature was then raised
3. 3
   温度to mild reflux
4. 4
   workup.DISSOLUTIONhad dissolved
5. 5
   温度heating
6. 6
   温度maintained for a further 24 hr
7. 7
   その他the precipitated sodium chloride removed by filtration
8. 8
   workup.DISSOLUTIONThe filtrate was dissolved in an excess of water
9. 9
   抽出extracted with four portions of 500 ml methylene chloride
10. 10
    乾燥the combined organic layers were dried over magnesium sulfate
11. 11
    その他The solvent was then removed by evaporation

実験手順

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.

出典