HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Bromobenzenesulfonyl chloride → 4-(4-BOC-piperazinosulfonyl)bromobenzene
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Bromobenzenesulfonyl chloride | HCID 7396 | — |
| Reactant | tert-Butyl piperazine-1-carboxylate | HCID 143452 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-(4-BOC-piperazinosulfonyl)bromobenzene | HCID 16665576 | 92.3% |
Reaction Steps
To a stirring, 0° C. solution of piperazine-1-carboxylic acid tert-butyl ester (1.17 g, 6.29 mmol, 1.05 equiv) and TEA (1.67 mL, 11.98 mmol, 2.0 equiv) in DCM (10 mL) was added 4-bromo-benzenesulfonyl chloride (1.53 g, 5.99 mmol, 1 equiv). The reaction was allowed to warm to ambient temperature and stir for 3 h. The reaction solvents were evaporated and the resulting solids were dried, washed with water and filtered, yielding a white powder (2.24 g, 92% yield). MS (ESI+): m/z=306.9, LC retention time: 3.17 min. Rf=0.56 (30% EtOAc/hexanes).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07456176B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-ce0b2feff8ab4fc6ade519a8285706be |
| Source note | uspto-grants-2008_11 |