Hydrochloric Acid → HCID 21188852, compound

HRID 1107017Notes

Reaction equation

HRID 1107017 reaction equation
[CH3:1][C:2]1[N:3]([CH2:10][CH2:11][N:12]([CH2:44][CH2:45][N:46]2[C:50]([N+:51]([O-:53])=[O:52])=[CH:49][N:48]=[C:47]2[CH3:54])[CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][N:21]([CH2:33][CH2:34][N:35]2[C:39]([N+:40]([O-:42])=[O:41])=[CH:38][N:37]=[C:36]2[CH3:43])[CH2:22][CH2:23][N:24]2[C:28]([N+:29]([O-:31])=[O:30])=[CH:27][N:26]=[C:25]2[CH3:32])[C:4]([N+:7]([O-:9])=[O:8])=[CH:5][N:6]=1.[ClH:55].CCOCC>CO>[ClH:55].[ClH:55].[CH3:32][C:25]1[N:24]([CH2:23][CH2:22][N:21]([CH2:33][CH2:34][N:35]2[C:39]([N+:40]([O-:42])=[O:41])=[CH:38][N:37]=[C:36]2[CH3:43])[CH2:20][CH2:19][CH2:18][CH2:17][CH2:16][CH2:15][CH2:14][CH2:13][N:12]([CH2:44][CH2:45][N:46]2[C:50]([N+:51]([O-:53])=[O:52])=[CH:49][N:48]=[C:47]2[CH3:54])[CH2:11][CH2:10][N:3]2[C:4]([N+:7]([O-:9])=[O:8])=[CH:5][N:6]=[C:2]2[CH3:1])[C:28]([N+:29]([O-:31])=[O:30])=[CH:27][N:26]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 9831995HCID 9831995, compound

Product 1

HCID 21188852HCID 21188852, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

N, N, N', N'-tetra[2'-(2-methyl-5-nitro-1-imidazolyl) ethyl]-1,8-octanediamine free base (1 g) is dissolved in 50 ml of warm methanol. To this solution, 5 ml of about 4 N ethanolic hydrochloric acid is added. Ether (20 ml) is then added slowly. The mixture solution is cooled and kept at 4° C. to facilitate precipitation. The precipitate is then collected by suction filtration, and recrystallized with methanol/ether to yield N, N, N', N'-tetra[2'-(2-methyl-5-nitro-1-imidazolyl) ethyl]-1,8-octanediamine-2HCl.

Workup

  1. temperatureThe mixture solution is cooled
  2. customkept at 4° C.
  3. customprecipitation
  4. filtrationThe precipitate is then collected by suction filtration
  5. customrecrystallized with methanol/ether

Sources & evidence

ORD record
ord-a15330c341e44e8e813ee61b1ba81c57
Source dataset
uspto-grants-2000_05
Patent number
US06057453

Reaction notes

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