反応 #7362

反応方程式

dimethyl carbonate

trimethyl amine

methanol

→

tetramethylammonium methyl-carbonate

収率 80.2%

反応条件

後処理

1. 1
   その他To a 1.5 L autoclave equipped with a stirrer
2. 2
   その他was sealed
3. 3
   温度Then the reaction mixture was cooled to 50° C.
4. 4
   その他discharged into a 1 L three-necked flask
5. 5
   その他Part of methanol was removed from the solution of tetramethylammonium methyl-carbonate in methanol
6. 6
   その他thus obtained under vacuum
7. 7
   温度the solution was cooled to ambient temperature
8. 8
   その他White crystal precipitated out
9. 9
   ろ過The crystal was filtrated
10. 10
    その他oven dried
11. 11
    その他recrystallized from methanol

実験手順

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%.

出典