Hampshire Chemical Corp.

Robert J Bulka

Gerald J O'Neill

Albert H Levesque

Felix B Popper

Process for the production of TMEDA in high yield by reducing 2,3-dimethyl-2,3-dinitrobutane with hydrogen in the presence of a chromium promoted Raney cobalt catalyst. A solution of 2,3-dimethyl-2,3-dinitrobutane in a suitable solvent is fed to a reactor while avoiding the accumulation of 2,3-dimethyl-2,3-dinitrobutane in the reaction medium, such as by feeding it at a rate no greater than its rate of reaction with hydrogen. In a preferred embodiment, the resulting TMEDA is recovered by converting it to an amine salt by sparging carbon dioxide through the solution.

Preparation of tetramethylethylenediamine

A process for the purification of bis(difluoromethyl)ether. Bis(difluoromethyl)ether is exposed to molecular sieves in order to reduce or completely remove impurities. In a further embodiment, the present invention optionally includes means for preferentially inhibiting the formation of CF.sub.2 HOCCl.sub.3 in the formation of bis(difluoromethyl)ether prior to exposing the bis(difluoromethyl)ether to the molecular sieves.

Purifications of flourinated dimethyl ethers

The synthesis of fluorinated dimethyl ethers of the formula CF.sub.2 HOCCl.sub.x F.sub.y H.sub.3-(x+y) wherein x is 0, 1 or 2; y is 1, 2 or 3; and wherein (x+y) is 1, 2 or 3. The process involves chlorination of methyl difluoromethyl ether in the presence of a solvent to form a chlorinated reaction product of the formula CF.sub.2 HOCH.sub.3-z Cl.sub.z wherein z is 1, 2 or 3. The process may also be carried out in the presence of oxygen in order to inhibit the formation of CF.sub.2 HOCCl.sub.3. The resulting compound(s) is then fluorinated with HF before or after separation, to give a fluorinated reaction product including the aforementioned fluorinated dimethyl ethers.

Chlorination of difluoromethyl methyl ether

A novel process for synthesizing difluoromethyl methyl ether for use as regrigerants and blowing agents, etc. is hereby disclosed. This process involves (1) feeding chlorodifluoromethane at a rate from about 0.5 to 5 grams of feed gas per gram of solution per minute through a sodium methoxide in methanol or basic ion exchange slurry in methanol; (2) removing the gaseous product and the unreacted chlorodifluoromethane continuously; and (3) separating difluoromethyl ether from the unreacted chlorodifluoromethane.

Synthesis of fluoromethyl ether

The synthesis of fluorinated dimethyl ethers of the formula CF.sub.2 HOCCl.sub.x F.sub.y H.sub.3-(x+y) wherein x is 0, 1 or 2; y is 1, 2 or 3; and wherein (x+y) is 1, 2 or 3. The process involves chlorination of methyl difluoromethyl ether in the presence of oxygen to form a chlorinated reaction product of the formula CF.sub.2 HOCH.sub.3-z Cl.sub.z wherein z is 1 or 2, and wherein the formation of CF.sub.2 HOCCl.sub.3 is inhibited. The resulting compound(s) is then fluorinated with HF before or after separation, to give a fluorinated reaction product including the aforementioned fluorinated dimethyl ethers.

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Merrimack, NH, United States of America

Robert J Bulka