تفاعل #7362

معادلة التفاعل

dimethyl carbonate

trimethyl amine

methanol

→

tetramethylammonium methyl-carbonate

المردود 80.2%

ظروف التفاعل

المعالجة

1. 1
   أخرىTo a 1.5 L autoclave equipped with a stirrer
2. 2
   أخرىwas sealed
3. 3
   درجة الحرارةThen the reaction mixture was cooled to 50° C.
4. 4
   أخرىdischarged into a 1 L three-necked flask
5. 5
   أخرىPart of methanol was removed from the solution of tetramethylammonium methyl-carbonate in methanol
6. 6
   أخرىthus obtained under vacuum
7. 7
   درجة الحرارةthe solution was cooled to ambient temperature
8. 8
   أخرىWhite crystal precipitated out
9. 9
   ترشيحThe crystal was filtrated
10. 10
    أخرىoven dried
11. 11
    أخرىrecrystallized from methanol

الإجراء التجريبي

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%.

المصدر