HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfamide → tert-Butyl 4-sulfamoylpiperazine-1-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfamide | HCID 82267 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | tert-Butyl 4-sulfamoylpiperazine-1-carboxylate | HCID 53628347 | 70% |
Reaction Steps
Sulfamide (5 eq) was added to a solution of tert-butyl piperazine-1-carboxylate in dioxane (0.12 M). The reaction was stirred at reflux overnight. The solvent was removed in vacuo, the residue taken up in EtOAc and washed with H2O, brine, before being dried (Na2SO4), filtered and concentrated in vacuo to give the crude material. Purification was by automated FC (EtOAc:PE:Et3N 40:60:0.02) to afford the title compound (70%). 1H NMR (300 MHz, DMSO-d6, 300 K) δ 1.39 (s, 9H), 2.88-2.90 (m, 4H), 3.37-3.39 (m, 4H), 6.78 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07989438B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-539387de13424ace964af61e5c608f91 |
| Source note | uspto-grants-2011_08 |