HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Methylpiperazine → 4-Methylpiperazine-1-sulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Methylpiperazine | HCID 53167 | — |
| Reactant | Sulfamide | HCID 82267 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 4-Methylpiperazine-1-sulfonamide | HCID 14326005 | — |
Reaction Steps
N-Methyl piperazine (5 ml) and sulfamide (11.26 g) in 1,4-dioxane (100 ml) were heated at reflux for 48 h. The solvent was evaporated under reduced pressure and the resulting solid dissolved in a mixture of methanol and water and applied to a plug of SCX-silica followed by further elution with aqueous methanol. This was then followed by elution with 1M ammonia in methanol (×4) and these fractions collected and solvent evaporated to dryness leaving a white solid. This was triturated with Et2O and filtered leaving the subtitle compound as a white solid. Yield: 5.0 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08106063B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-77e2a44ab5014a09837ea345ae6ae6d3 |
| Source note | uspto-grants-2012_01 |