Hydrochloric Acid → HCID 178492103, compound

HRID 1493331Notes

Reaction equation

HRID 1493331 reaction equation
C([NH:9][C:10]([NH:24][CH2:25][CH2:26][CH2:27][C:28]1[N:29]=[CH:30][NH:31][CH:32]=1)=[N:11][CH2:12][CH2:13][CH2:14][CH2:15][C:16]1[C:21]([O:22][CH3:23])=[CH:20][CH:19]=[CH:18][N:17]=1)(=O)C1C=CC=CC=1.[ClH:33]>O>[ClH:33].[ClH:33].[ClH:33].[CH3:23][O:22][C:21]1[C:16]([CH2:15][CH2:14][CH2:13][CH2:12][NH:11][C:10]([NH2:9])=[N:24][CH2:25][CH2:26][CH2:27][C:28]2[N:29]=[CH:30][NH:31][CH:32]=2)=[N:17][CH:18]=[CH:19][CH:20]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 178492102HCID 178492102, compound

Product 1

HCID 178492103HCID 178492103, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

0.75 g (1.7 mmol) of N1 -benzoyl-N2 -[4-(3-methoxy-pyridin-2-yl)butyl]-N3 -[3-(1H-imidazol-4-yl)propyl]guanidine and 15 ml of conc. hydrochloric acid are boiled under reflux for 18 hours. After cooling, the reaction mixture is diluted to 30 ml with water and extracted with 4×25 ml diethylether. The aqueous phase is then filtered and concentrated by evaporation under vacuum. The residue is taken up twice with 20 ml of absolute ethanol and again concentrated by evaporation. 0.74 g (98%) of a colourless, amorphous, highly hygroscopic solid is obtained.

Workup

  1. temperatureunder reflux for 18 hours
  2. temperatureAfter cooling
  3. extractionextracted with 4×25 ml diethylether
  4. filtrationThe aqueous phase is then filtered
  5. concentrationconcentrated by evaporation under vacuum
  6. concentrationagain concentrated by evaporation
  7. custom0.74 g (98%) of a colourless, amorphous, highly hygroscopic solid is obtained

Sources & evidence

ORD record
ord-79f3c9cffaf74785942b7f7e49fcce8d
Source dataset
uspto-grants-1991_06
Patent number
US05021431

Reaction notes

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