A method of forming a sucrose-6-ester includes in sequence the steps of: a) contacting sucrose with a organotin-based acylation promoter in a solvent in the presence of a base selected from amines and basic alkali metal salts; b) removing water to form a tin-sucrose adduct; and c) contacting the tin
A method of forming a sucrose-6-ester includes in sequence the steps of: a) contacting sucrose with a organotin-based acylation promoter in a solvent in the presence of a base selected from amines and basic alkali metal salts; b) removing water to form a tin-sucrose adduct; and c) contacting the tin-sucrose adduct with an acylating agent to form the sucrose-6-ester. The sucrose-6-ester may then be converted to sucralose.
대표청구항▼
1. A method of forming a sucrose-6-ester, comprising in sequence the steps of: a) contacting sucrose with an organotin-based acylation promoter selected from 1,3-diacyloxy-1,1,3,3-tetra-(hydrocarbyl)distannoxanes in a solvent in the presence of a base selected from the group consisting of sodium car
1. A method of forming a sucrose-6-ester, comprising in sequence the steps of: a) contacting sucrose with an organotin-based acylation promoter selected from 1,3-diacyloxy-1,1,3,3-tetra-(hydrocarbyl)distannoxanes in a solvent in the presence of a base selected from the group consisting of sodium carbonate, potassium carbonate, sodium hydroxide, sodium acetate and sodium phosphate dibasic;b) removing water of reaction to form a tin-sucrose adduct; andc) contacting the tin-sucrose adduct with an acylating agent to form the sucrose-6-ester;wherein the base is present in a range from 0.01 to 0.25 equivalents relative to the acylating agent. 2. The method of claim 1, wherein the base is present at a level in a range from 0.05 to 0.25 equivalents relative to the acylating agent. 3. The method of claim 1, wherein the base comprises sodium carbonate or potassium carbonate. 4. The method of claim 1, wherein the base comprises sodium acetate. 5. The method of claim 1, wherein the base comprises sodium phosphate dibasic. 6. The method of claim 1, wherein the base is present at a level in a range from 0.025 to 0.25 equivalents relative to the acylating agent. 7. The method of claim 1, wherein the base is present at a level in a range from 0.05 to 25 equivalents relative to the acylating agent. 8. The method of claim 1, wherein the organotin-based acylation promoter comprises 1,3-diacetoxy-1,1,3,3-tetrabutyldistannoxane. 9. The method of claim 1, wherein the organotin-based acylation promoter comprises 1,3-dibenzoyloxy-1,1,3,3-tetrabutyldistannoxane. 10. The method of claim 1, wherein the acylating agent comprises an acyl anhydride. 11. The method of claim 1, wherein the acylating agent comprises acetic anhydride. 12. The method of claim 1, wherein the acylating agent comprises benzoic anhydride. 13. The method of claim 1, wherein the solvent comprises a tertiary amide. 14. The method of claim 13, wherein the tertiary amide comprises dimethyl formamide. 15. The method of claim 1, wherein the solvent further comprises a solvent capable of forming an azeotrope with water. 16. The method of claim 15, wherein the solvent capable of forming an azeotrope with water comprises a hydrocarbon solvent. 17. A method of making sucralose, comprising in sequence the steps of: a) contacting sucrose with an organotin-based acylation promoter selected from 1,3-diacyloxy-1,1,3,3-tetra-(hydrocarbyl)distannoxanes in a solvent in the presence of a base selected from the group consisting of sodium carbonate, potassium carbonate, sodium hydroxide, sodium acetate and sodium phosphate dibasic;b) removing water of reaction to form a tin-sucrose adduct;c) contacting the tin-sucrose adduct with an acylating agent to form a sucrose-6-ester; andd) converting the sucrose-6-ester to sucralose and isolating and purifying the sucralose;wherein the base is present in a range from 0.01 to 0.25 equivalents relative to the acylating agent.
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