HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 4136951, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Diketene | HCID 12661 | — |
| Reactant | 4-Bromo-2-nitroaniline | HCID 70132 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 4136951 | HCID 4136951 | 74% |
Reaction Steps
A solution of diketene (0.32 ml, 4.15 mmol) in toluene (2 ml) was added to an 80° C. solution of 4-bromo-2-nitroaniline (900 mg, 4.15 mmol) in toluene (7 ml) and the solution was heated at reflux for 5 h. Triethylamine (0.58 ml, 4.15 mmol) in toluene (2 ml) was added and refluxing was continued for 30 min. The cooled solution was concentrated in vacuo and the crude product purified by column chromatography on silica gel eluting with 2:1 hexane/EtOAc to give the title compound as a yellow solid (920 mg, 74%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09095590B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-d1f47e4f40ed46ac82a314001efb18e2 |
| Source note | uspto-grants-2015_08 |