HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178505456, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 68157269 | HCID 68157269 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178505456 | HCID 178505456 | 85.5% |
Reaction Steps
(6-Fluoro-1-phenyl-1H-benzoimidazol-2-ylmethyl)[9-(tetrahydropyran-2-yl)-9H-purin-6-yl]amine (0.125 g, 0.28 mmol) in MeOH (2 mL) was treated with 4M HCl in dioxane (0.35 mL). After 15 min at 20° C. the reaction was poured onto a 10 g SCX cartridge which was eluted first with methanol then with 1:1 MeOH/2M NH3 in isopropanol. Product containing fractions were evaporated to a white solid. This was triturated with diethyl ether and dried to give 443 as a white solid, (86 mg, 85%). LCMS (Method C): RT 3.16 min [M+H]+ 360.02. NMR δ (ppm) (DMSO-d6): 12.9 (1H, s), 8.11 (2H, s), 7.92 (1H, s), 7.66-7.60 (6H, m), 7.09 (1H, td, J=9.31, 2.45 Hz), 6.93 (1H, dd, J=8.96, 2.50 Hz), 4.8 (2H, bs)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653089B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-25495d19e9ff47ce97b4990df5f33098 |
| Source note | uspto-grants-2014_02 |