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US 4,908,461 AGranted
Process for dechlorinating 4,5-dichlorofluorodioxolanes to obtain fluorodioxoles
AssigneeE. I. Du Pont de Nemours and Company
InventorMing-Hong Hung
Life of this patent
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Abstract
Process for preparing dioxoles by dechlorinating 4,5-dichlorodioxolanes with selected molar quantities of a lithium aluminum hydride/titanium (III or IV) chloride reagent at 20.degree.-35.degree. C.
Claims3
Dechlorination process for preparing the dioxole of the formula ##STR3## wherein R.sub.1 and R.sub.2 are each independently selected from the class consisting of fluorine, chloroalkyl, chlorofluoroalkyl and fluoroalkyl of 1-3 carbon atoms, and R.sub.3 is F, Cl or perfluoroalkyl of 1-3 carbon atoms, which process comprises:
- A. adding LiAlH.sub.4 and TiCl.sub.x wherein x is 3 or 4 to tetrahydrofuran at a molar ratio of LiAlH.sub.4 to TiCl.sub.x of 2:1 to 8:1, and mixing the components at 0.degree. C. to the reflux temperature of the mixture for 15-120 minutes;
- B. mixing the dioxolane of the formula ##STR4## wherein R.sub.1, R.sub.2 and R.sub.3 are as defined above into the mixture prepared in Step A until the molar ratio of the dioxolane to TiCl.sub.x is 1:1 to 4:1, at a temperature of 20.degree.-35.degree. C.;
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- C. isolating from Step B the dioxole of the aforesaid formula formed.
1 more element
Dependencies are inferred from the claim text.