HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178478976, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 178452207 | HCID 178452207 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 178478976 | HCID 178478976 | 95% |
Reaction Steps
A mixture of tert-butyl 4-(5-cyclopropyl-3-iodo-1H-pyrazolo[3,4-b]pyridin-4-yl)piperazine-1-carboxylate (200 mg, 0.426 mmol) and 4N HCl in dioxane (4 mL) was stirred at room temperature for 2 hours. The solvent was then removed in vacuo, and the residue was triturated with CH3CN. The solid formed was filtered, washed with Et2O and dried to provide 5-cyclopropyl-3-iodo-4-(piperazin-1-yl)-1H-pyrazolo[3,4-b]pyridine hydrochloride salt (179 mg, 95% yield) as a solid. 1H NMR (400 MHz, d6-DMSO) δ 9.47 (br s, 2H), 8.32 (s, 1H), 3.67-3.62 (m, 4H), 3.42-3.35 (m, 4H), 2.09-2.03 (m, 1H), 1.07-1.01 (m, 2H), 0.80-0.76 (m, 2H); LCMS (APCI+) m/z 370 (M+H)+, Retention time=1.87 minutes.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08372842B2 |
| Source dataset | uspto-grants-2013_02 |
| ORD ID | ord-11dd3864d064455cbf4597a101d2a46f |
| Source note | uspto-grants-2013_02 |