HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → (4-Bromo-1-methyl-1H-pyrazol-3-yl)-1-piperazinylmethanone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | tert-Butyl 4-(4-bromo-1-methyl-1H-pyrazole-3-carbonyl)piperazine-1-carboxylate | HCID 46901911 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | (4-Bromo-1-methyl-1H-pyrazol-3-yl)-1-piperazinylmethanone | HCID 46901601 | 100.1% |
Reaction Steps
4-(4-Bromo-1-methyl-1H-pyrazole-3-carbonyl)-piperazine-1-carboxylic acid tert-butyl ester (800 mg, 2.14 mmol) from Step A and HCl in dioxane (4 N, 5.36 mL) was stirred at room temperature for 1 h. The solvent was removed under reduced pressure to afford the hydrochloride salt of the title compound (585 mg) as a light yellow solid. 1H NMR (Acetonitrile-d3, 400 MHz) δ 3.20-3.26 (m, 4H), 3.92 (s, 3H), 3.98-4.05 (m, 4H), 7.71 (s, 1H), 9.40-9.50 (bs, 2H). Exact mass calculated for C9H13BrN4O: 272.0. Found: LCMS m/z (%)=273.0 (M+H+79Br, 100%), 275.0 (M+H+81Br, 97%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09434692B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-32fc4f4a57054be688c901f51cc62f2f |
| Source note | uspto-grants-2016_09 |