Methanol → Tetramethylammonium Methyl Carbonate

Temperature

140 °C

To a 1.5 L autoclave equipped with a stirrer and a heating means were added 90 g (1.0 mol) of dimethyl carbonate, 59 g (1.0 mol) of trimethyl amine and 510 g (15 mol) of methanol. Stirring was initiated after the autoclave was sealed. The autoclave was heat to 140° C., and pressure was 1.5 MPa. The reaction was kept at 140° C. for 4 h. Then the reaction mixture was cooled to 50° C. and discharged into a 1 L three-necked flask. Part of methanol was removed from the solution of tetramethyl ammonium methyl-carbonate in methanol thus obtained under vacuum, and then the solution was cooled to ambient temperature. White crystal precipitated out. The crystal was filtrated, oven dried and re-crystallized from methanol, to give 119.5 g of tetramethylammonium methyl-carbonate having a purity of 99.2% as measured by chromatography. The yield was 80.2%.

1. customTo a 1.5 L autoclave equipped with a stirrer
2. customwas sealed
3. temperatureThen the reaction mixture was cooled to 50° C.
4. customdischarged into a 1 L three-necked flask
5. customPart of methanol was removed from the solution of tetramethyl ammonium methyl-carbonate in methanol
6. customthus obtained under vacuum
7. temperaturethe solution was cooled to ambient temperature
8. customWhite crystal precipitated out
9. filtrationThe crystal was filtrated
10. customoven dried
11. customre-crystallized from methanol

ORD record

ord-cb7f7356772046b1839bdd7eaf8538c7

Source dataset

uspto-grants-2011_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07989662B2