Claims
- 1. A method for the preparation of trisodium phosphonoformate hexahydrate, comprising the steps of adding sodium hydroxide to water; heating the aqueous sodium hydroxide solution to 50.degree. C.; adding triethyl phosphonoformate to said solution at 50.degree. C. so as to produce a reaction mixture containing trisodium phosphonoformate and ethanol; heating the reaction mixture to reflux temperature for about 1 hour for removing the ethanol; cooling the reaction mixture to a temperature between about 17.degree. C. and about 30.degree. C.; and filtering off the product, trisodium phosphonoformate hexahydrate.
- 2. A method for the preparation of trisodium phosphonoformate hexahydrate, comprising the steps of adding sodium hydroxide to water; heating the aqueous sodium hydroxide solution to 50.degree. C.; adding triethyl phosphonoformate to said solution at 50.degree. C. so as to produce a reaction mixture; heating the reaction mixture to a temperature of 90.degree. C.-95.degree. C. for about 1 hour; cooling the reaction mixture of 20.degree. C.-30.degree. C.; and filtering off the crystalline product.
- 3. A method for the preparation of trisodium phosphonoformate hexahydrate, comprising the steps of adding sodium hydroxide to water, heating the aqueous sodium hydroxide solution to 50.degree. C., adding triethyl phosphonoformate to said solution at 50.degree. C. so as to produce a reaction mixture containing trisodium phosphonoformate acid and ethanol, heating the reaction mixture to a temperature of 90.degree. C.-95.degree. C. for about 1 hour so as to remove the ethanol, cooling the reaction mixture to about 20.degree. C. and filtering off the crystalline trisodium phosphonoformate product.
- 4. The method according to claim 1, 2, or 3 additionally comprising the subsequent steps of dissolving the product in water and then recrystallizing by cooling the solution to a temperature ranging from about 20.degree. C. to about 30.degree. C. so as to produce trisodium phosphonoformate hexahydrate.
- 5. The method according to any one of claims 1, 2 or 3 additionally comprising the subsequent steps of dissolving the product in water and then recrystallizing by cooling the solution to 20.degree. C. giving trisodium phosphonoformate hexahydrate.
- 6. The method according to claim 1 wherein the reflux temperature is about 90.degree. C. to about 95.degree. C.
- 7. A method for the preparation of crystalline trisodium phosphonoformate hexahydrate comprising the steps of
- (a) adding a suitable amount of sodium hydroxide to water so as to make an approximately 5.8M aqueous sodium hydroxide solution;
- (b) heating the aqueous sodium hydroxide solution to 50.degree. C.;
- (c) maintaining the aqueous sodium hydroxide solution at 50.degree. C. while admixing triethyl phosphonoformate at a molar ratio to sodium hydroxide of about 1:6 so as to produce a reaction mixture containing trisodium phosphonoformate and ethanol;
- (d) evaporating the ethanol by heating the admixture to a temperature range of about 90.degree. C. to about 95.degree. C. for a time sufficient to evaporate the ethanol;
- (e) cooling the admixture to a temperature of not less than about 17.degree. C. and no more than about 30.degree. C. so as to precipitate the crystalline trisodium phosphonoformate hexahydrate product; and
- (f) filtering off the crystalline product.
- 8. The method according to claim 7, wherein the admixture is cooled to a temperature range of about 20.degree. C. to about 25.degree. C.
Parent Case Info
This application is a continuation of application Ser. No. 08/091,475, filed Jul. 14, 1993 (abandoned), which is a continuation of application Ser. No. 07/773,621, filed as PCT/SE91/00172 Mar. 6, 1991 (abandoned).
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4018854 |
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Continuations (2)
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Number |
Date |
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91475 |
Jul 1993 |
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Parent |
773621 |
Nov 1991 |
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