HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178523893, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-Chlorobenzylamine | HCID 66036 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | HCID 178512031 | HCID 178512031 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 178523893 | HCID 178523893 | — |
Reaction Steps
To a stirred solution of N-[1-(2,4-dichlorophenyl)-2-(imidazol-1-yl)-ethyl]-N′-(4-chlorophenyl)guanidine of Example 231 (step B) in THF was added carbonyldimidazole. The reaction mixture was allowed to stir at rt for 2 h, then 4-chlorophenylmethylamine was added. This was allowed to stir at rt for 18 h. The solvent was removed and the residue partitioned between EtOAc and ammonium chloride solution. The organic layer was separated, dried, concentrated, and purified by silica gel column chromatography (EtOAc, MeOH, NH4OH; 90:10:0.1) to give an oil. The oil was dissolved in MEOH, and to this was added HCl solution in ether. The solvent was removed to give the title compound as a solid. MS (ES): r/z 576 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06916813B2 |
| Source dataset | uspto-grants-2005_07 |
| ORD ID | ord-49462e7e1f1d4fa4acbed03a9d538801 |
| Source note | uspto-grants-2005_07 |