Reaktion #1483082

Reaktionsgleichung

Formic acid

N-methyl-N-(2-propylheptyl)-amine

→

N-methyl-N-(2-propylheptyl)-formamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeequipped with a condenser
2. 2
   workup.ADDITIONadded drop wise to the round bottomed flange flask over a time period of 1 hour
3. 3
   Temperaturduring heating
4. 4
   Sonstigewas set to 180° C., while the boiling point
5. 5
   Sonstigereaction mixture
6. 6
   Sonstigewas ˜125° C
7. 7
   workup.DISTILLATIONWater was distilled off
8. 8
   Sonstigecollected in a round bottomed receiver flask
9. 9
   Sonstigeremoved from the reaction medium
10. 10
    SonstigeDuring the reaction the boiling point of the reaction medium
11. 11
    Sonstigewas performed at atmospheric pressure for a total time of 3.5 hours
12. 12
    Sonstigethe reaction
13. 13
    Sonstigethe remaining unreacted material was removed
14. 14
    Sonstigefor two hours

Vorschrift

A total amount of 846 g (4.81 moles) of N-methyl-N-(2-propylheptyl)-amine was added to a 2 l round bottomed flange flask equipped with a condenser. Formic acid was charged into a dropping funnel in an amount of 223.3 g (4.80 moles) and added drop wise to the round bottomed flange flask over a time period of 1 hour during heating and stirring with a magnetic stirrer. The final temperature was set to 180° C., while the boiling point of the initial reaction mixture was ˜125° C. Water was distilled off and collected in a round bottomed receiver flask and thereby removed from the reaction medium. During the reaction the boiling point of the reaction medium rose continuously. The reaction was performed at atmospheric pressure for a total time of 3.5 hours. Titration of remaining amine was performed to monitor the reaction. When the amine value did not decrease anymore, the remaining unreacted material was removed by gently pulling vacuum to 100 mbar for two hours. The reaction mixture was cooled to 60° C. before breaking the vacuum.

Quelle