Oxetane, 3,3-bis(chloromethyl)- → 3,3-Bis(methoxyethoxymethyl)oxetane

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.

1. customTo a 5 liter, three-neck flask, fitted with a reflux condenser, a stirrer
2. temperatureThe flask temperature was then raised
3. temperatureto mild reflux
4. dissolutionhad dissolved
5. temperatureheating
6. temperaturemaintained for a further 24 hr
7. customthe precipitated sodium chloride removed by filtration
8. dissolutionThe filtrate was dissolved in an excess of water
9. extractionextracted with four portions of 500 ml methylene chloride
10. dry with materialthe combined organic layers were dried over magnesium sulfate
11. customThe solvent was then removed by evaporation

ORDレコード

ord-ccdf9898e5a14564b4cd7599ca31a12f

出典データセット

uspto-grants-1988_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04764586