Process for the preparation of 1, 2-dichlorethane free crystals of zonisamide
View Patent ↗A process for the preparation of crystals of zonisamide containing residual 1,2-dichloroethane of not more than 5 ppm, by adding an aqueous C 2-4 alcohol to crystals of zonisamide containing residual 1,2-dichloroethane of more than 5 ppm, removing the 1,2-dichloroethane by azeotropic distillation, followed by collecting the precipitated crystals from the residual mixture.
1. A process for the preparation of crystals of 1,2-benzisoxazole-3-methanesulfonamide containing residual 1,2-dichloroethane of not more than 5 ppm, which comprises adding an aqueous C 2-4 alcohol to crystals of 1,2-benzisoxazole-3-methanesulfonamide containing residual 1,2-dichloroethane of more than 5 ppm, removing said 1,2-dichloroethane by azeotropic distillation to obtain a residual mixture, followed by collecting precipitated crystals of 1,2-benzisoxazole-3-methanesulfonamide containing not more than 5 ppm of 1,2-dichloroethane from the residual mixture.
2. A process for the preparation of crystals of 1,2-benzisoxazole-3-methanesulfonamide containing residual 1,2-dichloroethane of not more than 5 ppm, which comprises:
(a) dissolving crystals of 1,2-benzisoxazole-3-methanesulfonamide containing residual 1,2-dichloroethane of more than 5 ppm in an aqueous C 2-4 alcohol, and subjecting the resultant mixture to azeotropic distillation;
(b) stopping the distillation after the azeotropic distillation of said 1,2-dichloroethane is completed to obtain a residual mixture;
(c) cooling the residual mixture to precipitate crystals of 1,2-benzisoxazole-3-methanesulfonamide containing not more than 5 ppm of 1,2-dichloroethane; and
(d) collecting the precipitated crystals of 1,2-benzisoxazole-3-methanesulfonamide by filtration and drying thereof.
3. A process for the preparation of crystals of 1,2-benzisoxazole-3-methanesulfonamide containing residual 1,2-dichloroethane of not more than 5 ppm, which comprises:
(a) dissolving crystals of 1,2-benzisoxazole-3-methanesulfonamide containing residual 1,2-dichloroethane of more than 5 ppm in an aqueous C 2-4 alcohol, and subjecting the resultant mixture to azeotropic distillation;
(b) stopping the distillation after the azeotropic distillation of said 1,2-dichloroethane is completed to obtain a residual mixture;
(c1) adding the same C 2-4 alcohol as used in (a) and/or water to the residual mixture obtained in (b), dissolving the residual mixture with heating, and cooling thereof to precipitate crystals of 1,2-benzisoxazole-3-methanesulfonamide containing not more than 5 ppm of 1,2-dichloroethane; and
(d1) collecting the precipitated crystals of 1,2-benzisoxazole-3-methanesulfonamide by filtration and drying thereof.
4. The process according to claim 1 , wherein the aqueous C 2-4 alcohol is an aqueous isopropanol.
5. The process according to claim 1 , wherein the aqueous C 2-4 alcohol is isopropanol containing water in an amount of 35 to 65% by volume.
6. The process according to claim 2 , wherein the temperature at which the distillation is stopped is in the range of from 78° C. to 100° C.
7. A process for the preparation of crystals of 1,2-benzisoxazole-3-methanesulfonamide containing residual 1,2-dichloroethane of not more than 5 ppm, which comprises adding an aqueous C 2-4 alcohol to crystals of 1,2-benzisoxazole-3-methanesulfonamide containing residual 1,2-dichloroethane of more than 5 ppm and distilling the resulting mixture, to remove at least some of the residual 1,2-dichloroethane from the crystals of 1,2-benzisoxazole-3-methanesulfonamide containing residual 1,2-dichloroethane of more than 5 ppm.