HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetylacetone → 6-Bromo-2-methyl-4-nitro-1H-benzo[d]imidazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetylacetone | HCID 31261 | — |
| Reactant | 5-Bromo-3-nitrobenzene-1,2-diamine | HCID 45789403 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 6-Bromo-2-methyl-4-nitro-1H-benzo[d]imidazole | HCID 66976770 | 90% |
Reaction Steps
A mixture of 5-bromo-3-nitrobenzene-1,2-diamine (464 mg) and pentane-2,4-dione (400 mg) in EtOH (27 mL) and 5 N HCl (7.4 mL) was refluxed for 3 h. The mixture was cooled to room temperature and the solvent was removed in-vacuo. The residue was dissolved in EtOAc and washed with aqueous NaHCO3 solution and brine. The organic layer was concentrated to afford the desired product as a solid (460 mg, 90%). 1H NMR (300 MHz, CDCl3) δ ppm 2.73 (s, 3H), 8.11 (d, 1H, J=1.8 Hz), 8.24 (d, 1H, J=1.8 Hz), 10.20 (s, 1H, s); LC-MS: m/e=256 [M+1]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08865912B2 |
| Source dataset | uspto-grants-2014_10 |
| ORD ID | ord-513a91fa757d4071b3042484b277ced7 |
| Source note | uspto-grants-2014_10 |