HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 56648956, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Benzene-1,2-disulfonyl dichloride | HCID 246432 | — |
| Reactant | tert-Butyl (4-aminophenyl)carbamate | HCID 688611 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 56648956 | HCID 56648956 | — |
Reaction Steps
A solution of N-Boc-p-phenylenediamine (0.68 g, 3.26 mmol) and Et3N (0.51 mL, 7.19 mmol) in dry DCM (29 mL) was added to a refluxing solution of 1,2-benzenedisulfonyl dichloride (0.90 g, 3.27 mmol) in DCM (135 mL). After the addition was complete, the reaction solution was maintained at reflux for an additional 2 h. The heat was removed and after 16 h at rt, the solvent was removed under reduced pressure. The residue of the crude reaction mixture was dissolved in DCM and washed with saturated NaHCO3, brine, and dried. After filtration and concentration under reduced pressure yielding tert-butyl (4-(1,1,3,3-tetraoxidobenzo[d][1,3,2]dithiazol-2-yl)phenyl)carbamate, 1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08658650B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-19343db490584ac79a6c53e895365b7e |
| Source note | uspto-grants-2014_02 |