HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → 4-Methyl-2-(piperazin-1-yl)pyrimidine dihydrochloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | tert-Butyl 4-(4-methylpyrimidin-2-yl)piperazine-1-carboxylate | HCID 15132529 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | 4-Methyl-2-(piperazin-1-yl)pyrimidine dihydrochloride | HCID 18364978 | 71% |
Reaction Steps
The product from the previous step (tert-butyl 4-(4-methylpyrimidin-2-yl)piperazine-1-carboxylate) was dissolved in a one-to-one mixture of trifluoroacetic acid and DCM (8 ml) and stirred at room temperature for three hours. The volatiles were removed under reduced pressure, the residue was dissolved in DCM and evaporated. The residue was dissolved in THF (10 ml), HCl in dioxane (4N, 2 ml) was added and the resulting precipitate was collected by repeated centrifugation, dekantation and washing with THF to yield 107 mg of a solid (0.30 mmol, 71%). MS (APCI) m/z=179.1 [M+1]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09260441B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-157bd86215b644048653cf862e9d567b |
| Source note | uspto-grants-2016_02 |