Water → HCID 87127221, compound
Reaction equation
[CH2:1]([CH2:13][CH2:14][NH2:15])[CH2:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][NH2:12].[OH2:16].[F:17][C:18]([F:25])([F:24])[C:19]([O:21]CC)=O>C(#N)C>[F:25][C:18]([F:17])([F:24])[C:19]([NH:15][CH2:14][CH2:13][CH2:1][CH2:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][NH:12][C:19](=[O:16])[C:18]([F:25])([F:24])[F:17])=[O:21]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
Bis(hexamethylene)triamine (8.62 g, 40 mmol) was dissolved in acetonitrile (120 ml). Water (0.864 ml) was added to the mixture. Ethyl trifluoroacetate (16.7 ml, 140 mmol) was added to the mixture cooled in an ice bath. After addition, the mixture was refluxed for 16 hours. The solvents were removed by evaporation. The residue solidified upon storing at room temperature and was used for next step without purification.
Workup
- temperaturecooled in an ice bath
- additionAfter addition
- temperaturethe mixture was refluxed for 16 hours
- customThe solvents were removed by evaporation
- customupon storing at room temperature
- customwas used for next step without purification
Sources & evidence
- ORD record
- ord-394602d341d74c5d8a83247111f0d242
- Source dataset
- uspto-grants-2011_05
- Patent number
- US07935816B2
Reaction notes
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