Claims
- 1. The method for preparing sucralfate comprising:
- (a) reacting one equivalent of sucrose with at least 8 equivalents of chlorosulfonic acid which had been previously mixed and reacted with 2-picoline the latter at a temperature of about 40.degree.-50.degree. C. for from 1 to 2 hours;
- (b) adding aqueous ammonia at a temperature below 25.degree. C. to bring the pH of the reaction mixture to about 7.5-8.0;
- (c) adding an excess of methanol, ethanol or 2-propanol to separate sucrose octasulfate ammonium salt;
- (d) purifying said separated salt by recrystallization from aqueous ethyl alcohol;
- (e) reacting said salt with aluminum chlorohydrate in an alcoholic solvent at a molar ratio of approximately 1:8;
- (f) allowing said reaction to go to completion at ambient temperature and the product to separate;
- (g) purifying said product by washing with water to produce said product in water moist form; and
- (h) drying said moist form to produce a powder product form.
- 2. The method of claim 1 in which said sucrose octasulfate ammonium salt is not isolated and purified but is used directly in step (e).
- 3. The method of preparing sucralfate comprising adding sucrose octasulfate ammonium salt to at least 8 equivalents of aluminum chlorohydrate in an alcoholic solvent at ambient temperature.
- 4. The method of claim 3 in which the alcoholic solvent is ethanol.
- 5. The method of claim 3 in which the alcoholic solvent is aqueous ethanol.
- 6. The method of claim 5 in which no excess over 8 equivalents of aluminum chlorohydrate is used.
- 7. The method of claim 3 in which the separated sucralfate is maintained in water moist form and further used directly to prepare liquid oral dosage unit pharmaceutical forms.
- 8. The method of claim 3 in which said sucralfate has, or is sized to have, a particle size below 30 microns.
- 9. The method of claim 8 in which said particle size is from 5-10 microns.
- 10. The method of claim 3 in which the separated sucralfate is purified by washing with water.
- 11. The method of claim 3 in which vigorous stirring is used during the reaction.
- 12. The method of claim 3 in which the addition is slowly over a period of from 1-3 hours at ambient temperature.
- 13. The method of claim 3 in which the sucralfate is separated and heat dried.
- 14. The method of claim 3 in which the product sucralfate is formulated into a liquid or solid oral dosage unit composition.
- 15. The method of claim 3 in which the product sucralfate is formulated into an oral suspension product form which has an aqueous base with a gum sufficient to impart greater than aqueous viscosity and a sweetening agent.
- 16. The method of claim 15 in which the sweetening agent is sucrose and the gum is hydroxypropylmethyl cellulose.
- 17. In the method of preparing sucrose octasulfate by reacting sucrose with at least 8 molar equivalents of chlorosulfonic acid, the improvement comprising the use of 2-picoline as reactant-solvent.
Parent Case Info
This application is a continuation-in-part of Ser. No. 236,167, filed Aug. 25, 1988, now abandoned.
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Continuation in Parts (1)
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Number |
Date |
Country |
Parent |
236167 |
Aug 1988 |
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