HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178463570, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 68157935 | HCID 68157935 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178463570 | HCID 178463570 | 69.2% |
Reaction Steps
4N HCl in dioxane (0.5 mL) was added to a solution of [(S)-1-(7-chloro-6-fluoro-1-phenyl-1H-benzoimidazol-2-yl)ethyl]-[9-(tetrahydropyran-2-yl)-9H-purin-6-yl]amine (166 mg, 0.34 mmol) in MeOH (5 mL) and the mixture was stirred at RT for 1 h. The volatiles were removed in vacuo and the resulting residue was purified by HPLC (Phenomenex Gemini 5 μm C18 on a 25 min gradient 10-90%, 0.1% HCO2H in acetonitrile/water) to afford 179 (96 mg, 69%). LCMS (Method K): RT 3.80 min [M+H]+ 408.0/409.9/411.08. 1H NMR (DMSO-d6, 400 MHz): δ 8.22-7.83 (3H, m), 7.69-7.34 (6H, m), 7.33-7.24 (1H, t, J=9.50 Hz), 5.25 (1H, s), 1.56 (3H, d, J=6.88 Hz)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653089B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-43fe6d1464e64124958251dae4d2669e |
| Source note | uspto-grants-2014_02 |