HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 1-(3-Methyl-5-nitro-pyridin-2-yl)-piperazine hydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 4-(3-Methyl-5-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester | HCID 68537004 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 1-(3-Methyl-5-nitro-pyridin-2-yl)-piperazine hydrochloride | HCID 68537999 | 97% |
Reaction Steps
Add a solution of HCl 4M in dioxane (4 equiv) to a solution of 4-(3-Methyl-5-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (7.77 g, 24.13 mmol) in DCM (73 mL). Stir mixture at room temperature overnight. Add 2 more equiv of the HCl in dioxane solution. After no starting material is detected by LCMS, filter solid and dry under reduced pressure to obtain 6.91 g of 1-(3-methyl-5-nitro-pyridin-2-yl)-piperazine hydrochloride as a yellowish solid (97% yield). ES+(m/z): 259 [M+1].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652015B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-b4519c1e0f164db8b4c934a980f7b485 |
| Source note | uspto-grants-2010_01 |