Hydrochloric Acid → HCID 178478850, compound

HRID 1244975Notes

Reaction equation

HRID 1244975 reaction equation
[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH2:8])[CH2:4][CH2:3]1.[Cl:9][C:10]1[N:18]=[C:17]2[C:13]([N:14]=[CH:15][N:16]2[CH:19]2[CH2:23][CH2:22][CH2:21][CH2:20]2)=[C:12]([NH:24][C:25]2[CH:26]=[C:27]([CH:31]=[CH:32][CH:33]=2)[C:28]([NH2:30])=[O:29])[N:11]=1.CO.[OH-].[NH4+].[ClH:38]>CO>[ClH:9].[ClH:38].[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:10]2[N:18]=[C:17]3[C:13]([N:14]=[CH:15][N:16]3[CH:19]3[CH2:20][CH2:21][CH2:22][CH2:23]3)=[C:12]([NH:24][C:25]3[CH:26]=[C:27]([CH:31]=[CH:32][CH:33]=3)[C:28]([NH2:30])=[O:29])[N:11]=2)[CH2:4][CH2:3]1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 21894508Ammonium hydroxide methanolHCID 21922945HCID 21922945, compoundHCID 178511674HCID 178511674, compound

Product 1

HCID 178478850HCID 178478850, compound

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

400 mg of trans-1,4-diaminocyclohexane and 250 mg of the product obtained in Stage 1 above are taken to approximately 150° C., the reaction medium is left under agitation for 5 hours then left to return to ambient temperature for 16 hours. 8 ml of methanol is added, chromatography on silica is carried out (eluent: MeOH/NH4OH 98/2). The residue is taken up in an ethanolic solution of hydrochloric acid, followed by evaporating the solvents, impasting in ether, separating, drying under reduced pressure at ambient temperature and 101 mg of expected product is recovered.

Workup

  1. customabove are taken to approximately 150° C.
  2. waitthen left
  3. waitto return to ambient temperature for 16 hours
  4. customby evaporating the solvents
  5. customseparating
  6. customdrying under reduced pressure at ambient temperature
  7. custom101 mg of expected product is recovered

Sources & evidence

ORD record
ord-60ceebfb61e049a292f40909624d3510
Source dataset
uspto-grants-2006_10
Patent number
US07122669B1

Reaction notes

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