HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Hexyl 2-[[[4-[[4-[(dipropylamino)methyl]phenyl]carbamoyl]phenyl]methyl-[(1-hexoxycarbonylimidazol-2-yl)methyl]amino]methyl]imidazole-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hexyl chloroformate | HCID 22466 | — |
| Reactant | 4-{[bis(1H-imidazol-2-ylmethyl)-amino]-methyl}-N-(4-dipropylaminomethylphenyl)-benzamide | HCID 9983420 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | Hexyl 2-[[[4-[[4-[(dipropylamino)methyl]phenyl]carbamoyl]phenyl]methyl-[(1-hexoxycarbonylimidazol-2-yl)methyl]amino]methyl]imidazole-1-carboxylate | HCID 58801928 | — |
Reaction Steps
The compound obtained in Example 19-3 was treated with an anion-exchange resin. The treated product was dissolved in chloroform (4.0 ml) and added with n-hexyl chloroformate (manufactured by Tokyo Kasei Kogyo Co., Ltd.) (0.054 ml) and triethylamine (0.060 ml), followed by stirring at room temperature for 16 hours. After completion of the reaction, the solvent was distilled off. The residue was added with chloroform, washed with water and saturated saline solution, and dried with anhydrous sodium sulfate, followed by distilling the solvent off. Subsequently, the residue was purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (66.6 mg) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07176227B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-8e4fce9351804670beee69cf915a10f1 |
| Source note | uspto-grants-2007_02 |