HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 86681239, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pyrazole | HCID 1048 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | 4-Iodopyridin-2-amine | HCID 22607551 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 86681239 | HCID 86681239 | 90% |
Reaction Steps
A 20 mL reaction vessel was charged with 4-iodopyridin-2-amine (1.5 g, 6.8 mmol) and 1H-pyrazole (4.0 g, 58.9 mmol). Concentrated hydrochloric acid (1.5 ml) and 1,4-dioxane (1.5 mL) were added, and the reaction vessel was sealed. The mixture was irradiated in a microwave oven at 120° C. for 45 min and then at 130° C. for 60 min. The mixture was cooled to rt and then diethyl ether (6 ml) and ethanol (3 ml) were added. The mixture was sonicated for 10 min, and the solid was collected by filtration and washed with diethyl ether and n-hexane to give 4-(1H-pyrazol-1-yl)pyridin-2-amine hydrochloride (1.2 g, 90%) as a white solid. LCMS (ESI) m/z 161 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08952058B2 |
| Source dataset | uspto-grants-2015_02 |
| ORD ID | ord-5e73e4fd5ffb47f782b51cb311cd82b4 |
| Source note | uspto-grants-2015_02 |