Reaction equation
[NH2:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][NH:7][CH2:8][CH2:9][NH2:10].C([Cl:30])(=O)CCCCCCC/C=C\CCCCCCCC>ClCCl>[ClH:30].[ClH:30].[NH2:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][NH:7][CH2:8][CH2:9][NH2:10]Participants
5
Reactant 2
Product 2
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 5 °C
Procedure
1.12 g (7.5 mmol) of triethylenetetramine was added to 25 mL of dichloromethane and dissolved with stirring in an ice water bath at 5° C. for 30 minutes. To the solution, a solution of 2.00 g (6.0 mmol) of oleoyl chloride in 20 mL of dichloromethane in a separate reactor was added slowly dropwise while it was allowed to react at 5° C. for 3 hours. Due to hydrogen chloride produced during the reaction, unreacted triethylenetetramine HCl was precipitated. Before the end of the reaction, the upper layer solution was taken and analyzed by thin layer chromatography (TLC) with a mobile phase of ethanol:chloroform (2:1) to determine whether the reaction was completed.
Workup
- dissolutiondissolved
- customto react at 5° C. for 3 hours
Sources & evidence
- ORD record
- ord-c201cbd9f9124ceaa84143412cdaf34c
- Source dataset
- uspto-grants-2016_09
- Patent number
- US09439856B2
Linked notes
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