HCID 178469002, compound → HCID 178469003, compound

HRID 1824454Notes

Reaction equation

HRID 1824454 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[NH:11][C:12]([NH:19][C:20]2[CH:30]=[CH:29][C:23]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:22][CH:21]=2)=[C:13]2[C:17]([N:18]=1)=[N:16][CH:15]=[N:14]2>C(Cl)Cl.CO>[ClH:9].[ClH:9].[NH2:1][C@H:2]1[CH2:7][CH2:6][C@H:5]([NH:8][C:10]2[NH:11][C:12]([NH:19][C:20]3[CH:21]=[CH:22][C:23]([C:24]([O:26][CH2:27][CH3:28])=[O:25])=[CH:29][CH:30]=3)=[C:13]3[C:17]([N:18]=2)=[N:16][CH:15]=[N:14]3)[CH2:4][CH2:3]1

Participants

4

Reactant 2

HCID 178469002HCID 178469002, compoundHCID 178511674HCID 178511674, compound

Product 1

HCID 178469003HCID 178469003, compound

Reagents, catalysts & solvents 1

HCID 21226129Dichloromethane methanolSolvent

Procedure

970 mg of trans-1,4-diaminocyclohexane are heated to its melting point (70° C.), 269 mg of the product obtained in stage 1 above are added and the medium is then heated at 140–145° C. for 4 hours. The medium is allowed to return to room temperature and it is taken up in 50 ml of a CH2Cl2-methanol: 80-20 mixture. The medium is washed twice with 20 ml of H2O and once with 20 ml of sodium chloride as a saturated aqueous solution. The medium is dried over Na2SO4 and evaporated to dryness.

Workup

  1. additionabove are added
  2. temperaturethe medium is then heated at 140–145° C. for 4 hours
  3. customto return to room temperature
  4. washThe medium is washed twice with 20 ml of H2O and once with 20 ml of sodium chloride as a saturated aqueous solution
  5. dry with materialThe medium is dried over Na2SO4
  6. customevaporated to dryness

Sources & evidence

ORD record
ord-5fc96261448840c7a8846cd33dab41b0
Source dataset
uspto-grants-2006_05
Patent number
US07041824B2

Reaction notes

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