Water → HCID 87127221, compound

HRID 474135Notes

Reaction equation

HRID 474135 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

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

  1. temperaturecooled in an ice bath
  2. additionAfter addition
  3. temperaturethe mixture was refluxed for 16 hours
  4. customThe solvents were removed by evaporation
  5. customupon storing at room temperature
  6. customwas used for next step without purification

Sources & evidence

ORD record
ord-1ccd86bafac14801ae9c250c3f61d7e7
Source dataset
uspto-grants-2014_01
Patent number
US08637492B2

Reaction notes

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