反应详情

Under a nitrogen atmosphere, the reaction mixture from above is decanted into a clean, dry reaction vessel, leaving the unreacted magnesium turnings in the first vessel. This solution containing 2,2,3,3-tetrafluoro-2,3-dihydrobenzofuran-7-ylmagnesium chloride is heated at reflux, and 16.5 grams (0.55 mole based on formaldehyde) of polyoxymethylene diacetate (avg. mol. wgt. approx. 50,000, commercially available from E.I du Pont De Nemours & Co., Inc. Wilmington Del., under the trade name Delrin 500 acetal homopolymer resin), milled to about 80 mesh, is added with stirring during about a three hour period. Upon completion of addition, the reaction mixture is heated at reflux for an additional four hours and then is allowed to cool to ambient temperature as it stood for about 18 hours. The reaction mixture is warmed to about 53° C. and then is poured into 100 grams of ice, 52 grams of concentrated hydrochloric acid, and 200 grams of a mixture of 95% n-octane and 5% toluene (wt/wt). This mixture is filtered, and the organic layer is separated. The organic layer is concentrated under reduced pressure, yielding 2,2,3,3-tetrafluoro-2,3-dihydrobenzofuran-7-ylmethanol.

1. customUnder a nitrogen atmosphere, the reaction mixture from above is decanted into a clean,
2. customdry
3. customreaction vessel
4. temperatureis heated
5. temperatureat reflux
6. additionis added
7. additionUpon completion of addition
8. temperaturethe reaction mixture is heated
9. temperatureat reflux for an additional four hours
10. waitstood for about 18 hours
11. temperatureThe reaction mixture is warmed to about 53° C.
12. filtrationThis mixture is filtered
13. customthe organic layer is separated
14. concentrationThe organic layer is concentrated under reduced pressure