Method of making a templating agent
View Patent ↗A method for preparing 1-adamantyltrimethylammonium methylcarbonate or N,N-dimethyl-3,5-dimethylpiperidinium methylcarbonate is disclosed. The method comprises reacting dimethyl carbonate and 3,5-dimethylpiperidine or a 1-adamantylamine compound and in the presence of water in a sealed vessel at a temperature of from 80 to 200° C. The 1-adamantylamine compound is 1-adamantylamine, 1-adamantylmethylamine, or mixtures thereof.
1. A method for preparing N,N-dimethyl-3,5-dimethylpiperidinium methylcarbonate, comprising reacting dimethyl carbonate and 3,5-dimethylpiperidine in the presence of water in a sealed vessel at a temperature of from 80 to 200° C.
2. The method of claim 1 wherein the molar ratio of dimethyl carbonate: 3,5-dimethylpiperidine is in the range of 5 to 20.
3. The method of claim 1 wherein the molar ratio of dimethyl carbonate: 3,5-dimethylpiperidine is in the range of 8 to 14.
4. The method of claim 1 wherein the molar ratio of water: 3,5-dimethylpiperidine is in the range of 1 to 4.
5. The method of claim 1 wherein the reaction of 3,5-dimethylpiperidine with dimethyl carbonate is performed at a temperature in the range of 120-160° C.
6. The method of claim 1 further comprising reacting the N,N-dimethyl-3,5-dimethylpiperidinium methylcarbonate with calcium hydroxide in the presence of a water to produce 1N,N-dimethly-3,-5-dimethlypiperidinium hydroxide.
7. The method of claim 6 wherein the molar ratio of calcium hydroxide: N,N-dimethyl-3,5-dimethylpiperidinium methylcarbonate is in the range of 1.05 to 1.75.
8. The method of claim 7 wherein the reaction of N,N-dimethyl-3,5-dimethylpiperidinium methylcarbonate with calcium hydroxide in the presence of water is performed at reflux.