HCID 178487298, compound → HCID 178487299, compound
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][NH:16]2)=[C:12]([N:19]2[C:23]3[CH:24]=[CH:25][C:26]([O:28][CH3:29])=[CH:27][C:22]=3[N:21]=[CH:20]2)[N:11]=1>CS(C)=O>[ClH:9].[ClH:9].[CH3:29][O:28][C:26]1[CH:25]=[CH:24][C:23]2[N:19]([C:12]3[N:11]=[C:10]([NH:1][C@H:2]4[CH2:7][CH2:6][C@H:5]([NH2:8])[CH2:4][CH2:3]4)[N:18]=[C:17]4[C:13]=3[N:14]=[CH:15][NH:16]4)[CH:20]=[N:21][C:22]=2[CH:27]=1Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 120 °C
Procedure
969 mg of trans-1,4-diaminocyclohexane are brought to its melting temperature (70° C.), 5100 mg of product obtained in stage 1 above (no name) and 10 ml of DMSO are added in a single step, and the mixture is then heated at 120° C. for approximately 72 hours. The mixture is allowed to return to ambient temperature. Purification is carried out by chromatography on silica with an MeOH—NH4OH: 98-2 mixture for eluent. The purified product is dissolved in ethanol and HCl-AcOEt is then added. Partial drying and drying under vacuum at 60° C. are carried out. Purification is carried out by chromatography on silica with a CH2Cl2-MeOH—NH4OH: 75-23-2 mixture for eluent. 258 mg of expected product are obtained, in the form of beige-colored crystals.
Workup
- additionare added in a single step
- customto return to ambient temperature
- customPurification
- dissolutionThe purified product is dissolved in ethanol
- additionHCl-AcOEt is then added
- customPartial drying
- customdrying under vacuum at 60° C.
- customPurification
Sources & evidence
- ORD record
- ord-4f02d62e2cde48e0b43783ce84351300
- Source dataset
- uspto-grants-2009_01
- Patent number
- US07476670B2
Reaction notes
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