반응 #7362

반응 방정식

dimethyl carbonate

trimethyl amine

methanol

→

tetramethylammonium methyl-carbonate

수율 80.2%

반응 조건

후처리

1. 1
   기타To a 1.5 L autoclave equipped with a stirrer
2. 2
   기타was sealed
3. 3
   온도Then the reaction mixture was cooled to 50° C.
4. 4
   기타discharged into a 1 L three-necked flask
5. 5
   기타Part of methanol was removed from the solution of tetramethylammonium methyl-carbonate in methanol
6. 6
   기타thus obtained under vacuum
7. 7
   온도the solution was cooled to ambient temperature
8. 8
   기타White crystal precipitated out
9. 9
   여과The crystal was filtrated
10. 10
    기타oven dried
11. 11
    기타recrystallized from methanol

실험 절차

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%.

출처