Reaktion #7362

Reaktionsgleichung

dimethyl carbonate

trimethyl amine

methanol

→

tetramethylammonium methyl-carbonate

Ausbeute 80.2%

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 1.5 L autoclave equipped with a stirrer
2. 2
   Sonstigewas sealed
3. 3
   TemperaturThen the reaction mixture was cooled to 50° C.
4. 4
   Sonstigedischarged into a 1 L three-necked flask
5. 5
   SonstigePart of methanol was removed from the solution of tetramethylammonium methyl-carbonate in methanol
6. 6
   Sonstigethus obtained under vacuum
7. 7
   Temperaturthe solution was cooled to ambient temperature
8. 8
   SonstigeWhite crystal precipitated out
9. 9
   FiltrationThe crystal was filtrated
10. 10
    Sonstigeoven dried
11. 11
    Sonstigerecrystallized from methanol

Vorschrift

To a 1.5 L autoclave equipped with a stirrer and a heating means were added 90 g (11.0 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 tetramethylammonium 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 recrystallized 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%.

Quelle