Reaction #1483082

Reaction equation

Formic acid

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

→

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

Conditions

Workup

1. 1
   Otherequipped with a condenser
2. 2
   workup.ADDITIONadded drop wise to the round bottomed flange flask over a time period of 1 hour
3. 3
   Temperatureduring heating
4. 4
   Otherwas set to 180° C., while the boiling point
5. 5
   Otherreaction mixture
6. 6
   Otherwas ˜125° C
7. 7
   workup.DISTILLATIONWater was distilled off
8. 8
   Othercollected in a round bottomed receiver flask
9. 9
   Otherremoved from the reaction medium
10. 10
    OtherDuring the reaction the boiling point of the reaction medium
11. 11
    Otherwas performed at atmospheric pressure for a total time of 3.5 hours
12. 12
    Otherthe reaction
13. 13
    Otherthe remaining unreacted material was removed
14. 14
    Otherfor two hours

Procedure

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.

Source