HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 22272483, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 22272502 | HCID 22272502 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 22272483 | HCID 22272483 | 48% |
Reaction Steps
tert-Butyl 4-{4-(anilinosulfonyl)-2-[(methylsulfonyl)amino]phenyl}-1,4-diazepane-1-carboxylate (0.077 g, 0.147 mmol) was dissolved in MeOH, and ether saturated with HCl gas was added. The mixture was stirred at room temperature for 4 h and then concentrated. The crude solid was dissolved in a small amount of MeOH, and ether was added. The precipitate was collected and dried to give 30 mg of the pure product as the HCl salt (yield 48%): 1H NMR (DMSO-d6) δ 7.72–7.70 (m, 1H), 7.46–7.42 (m, 1H), 7.25–7.20 (m, 3H), 7.14–7.09 (m, 2H), 7.03–6.99 (m, 1H), 3.45–3.15 (m, partly obscured by solvent signal, HDO, 6H), 2.96 (s, 3H), 2.02–1.95 (m, 2H); MS (posES-FIA) m/z=425 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07173035B2 |
| Source dataset | uspto-grants-2007_02 |
| ORD ID | ord-4b57f3de1a9a4801b8cdf03f1d0971dc |
| Source note | uspto-grants-2007_02 |