HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 22063817, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | HCID 22063951 | HCID 22063951 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 22063817 | HCID 22063817 | 139% |
Reaction Steps
To a stirred solution of N-[4-(3-chloro-phenyl)-5-(1-cyclopentyl-3-methyl-2-oxo-2,3-dihydro-1H-benzoimidazol-5-yl)-1H-imidazol-2-yl]-acetamide (prepared as described above, 102 mg) in methanol:water (1:1, 10 mL) was added concentrated sulfuric acid (ca. 0.5 mL). The mixture was heated to reflux for 4 hours, after which the reaction was cooled to room temperature and the concentrated in vacuo. The resulting aqueous solution was diluted with water and the pH was adjusted to 10 with aqueous ammonium hydroxide. The mixture was filtered and the resulting white powder was taken up in 1M HCl in ether and concentrated in vacuo to afford 70 mg of the title compound as the HCl salt. MS (M+1)=408.1 (free base).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07056918B2 |
| Source dataset | uspto-grants-2006_06 |
| ORD ID | ord-f76b1117b2604937961cc1002b9567f4 |
| Source note | uspto-grants-2006_06 |