Formaldehyde → 1-Butanamine, N-butyl-N-methyl-
Reaction equation
[CH2:1]([NH:5][CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[CH2:10]=O>>[CH3:10][N:5]([CH2:6][CH2:7][CH2:8][CH3:9])[CH2:1][CH2:2][CH2:3][CH3:4]Participants
3
Procedure
In a similar manner to Example 1, 258.5 g (2.0 mol) of di-n-butylamine and 330.2 g (3.2 mol) of formaldehyde (29.1%) are reacted in a 1 l autoclave; a maximum pressure of 3.2 MPa is established at a temperature of 120° C. After the crude amine (aqueous and organic phase) has been degassed at a maximum temperature of 80° C., the water is removed on a water separator. The remaining organic phase is subsequently fractionally distilled. 274.6 g of N-methyldi-n-butylamine having a purity of 99.6% are isolated, corresponding to a yield of 95.6% of theory.
Workup
- customis established at a temperature of 120° C
- customAfter the crude amine (aqueous and organic phase) has been degassed at a maximum temperature of 80° C.
- customthe water is removed on a water separator
- distillationThe remaining organic phase is subsequently fractionally distilled
Sources & evidence
- ORD record
- ord-83ecc5200c54442981c68e3a50747494
- Source dataset
- uspto-grants-2006_01
- Patent number
- US06982352B2
Reaction notes
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