Method for synthesis of N-methyl piperazine diphenolamide and related composition
A method for synthesis of N-methyl piperazine diphenolamide is presented. The method includes contacting diphenolic acid with N-methyl piperazine to form a reaction mixture; and heating the reaction mixture to form a reaction product including N-methyl piperazine diphenolamide. An associated composition is also presented.
1. A method for synthesis of N-methyl piperazine diphenolamide, comprising:
contacting diphenolic acid with N-methyl piperazine to form a reaction mixture; and heating the reaction mixture to form a reaction product comprising N-methyl piperazine diphenolamide.
2. The method of claim 1 , wherein diphenolic acid is contacted with N-methyl piperazine under substantially solvent-free conditions.
3. The method of claim 1 , wherein a molar ratio of N-methyl piperazine to diphenolic acid is in a range from about 1.5 to about 5.
4. The method of claim 1 , wherein a molar ratio of N-methyl piperazine to diphenolic acid is in a range from about 3 to about 4.
5. The method of claim 1 , comprising heating the reaction mixture at a temperature in a range from about 140° C. to about 180° C. for a time duration in a range from about 8 hours to about 40 hours.
6. The method of claim 1 , comprising heating the reaction mixture at a temperature in a range from about 160° C. to about 180° C. for a time duration in a range from about 16 hours to about 24 hours.
7. The method of claim 1 , further comprising isolating N-methyl piperazine diphenolamide from the reaction product by crystallization.
8. The method of claim 1 , wherein N-methyl piperazine diphenolamide has a purity greater than about 98%.
9. The method of claim 1 , wherein the reaction product is substantially free of diphenolic acid methyl ester.
10. The method of claim 1 , wherein a yield of N-methyl piperazine diphenolamide relative to diphenolic acid is greater than about 80%.
11. A method for synthesis of N-methyl piperazine diphenolamide, comprising:
contacting diphenolic acid with N-methyl piperazine under substantially solvent free conditions to form a reaction mixture; and
heating the reaction mixture at a temperature in a range from about 160° C. to about 180° C. for a time duration in a range from about 16 hours to about 24 hours, to form a reaction product comprising N-methyl piperazine diphenolamide.
12. The method of claim 11 , wherein a molar ratio of N-methyl piperazine to diphenolic acid is in a range from about 1.5 to about 5.
13. The method of claim 11 , wherein a molar ratio of N-methyl piperazine to diphenolic acid is in a range from about 3 to about 4.
14. A composition comprising N-methyl piperazine diphenolamide, formed by:
contacting diphenolic acid with N-methyl piperazine to form a reaction mixture; and heating the reaction mixture to form a reaction product comprising the N-methyl piperazine diphenolamide.
15. The composition of claim 14 , wherein the composition is substantially free of diphenolic acid methyl ester.
16. The composition of claim 14 , wherein N-methyl piperazine diphenolamide has a purity greater than about 98%.
17. The composition of claim 14 , formed by contacting about 1.5 moles to about 5 moles of N-methyl piperazine relative to 1 mole of diphenolic acid.
18. The composition of claim 14 , formed by contacting about 3 moles to about 4 moles of N-methyl piperazine relative to 1 mole of diphenolic acid.
19. The composition of claim 14 , formed by heating the reaction mixture at a temperature in a range from about 140° C. to about 180° C. for a time duration in a range from about 8 hours to about 40 hours.
20. The composition of claim 14 , formed by heating the reaction mixture at a temperature in a range from about 160° C. to about 180° C. for a time duration in a range from about 16 hours to about 24 hours.