HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → 2-Chloro-5,6-dinitrobenzimidazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 5,6-Dinitro-2-benzoimidazolone | HCID 312775 | — |
| Product | 2-Chloro-5,6-dinitrobenzimidazole | HCID 267810 | 64.7% |
Reaction Steps
As represented in the following synthesis scheme, 10 g of 2-benzoimidazolone was heated and stirred in 100 mL of nitric acid (1.38) at 70° C. for 1 hour, followed by diluting with cold water, to thereby obtain yellow green 5,6-dinitro-2-benzoimidazolone (yield 76.5%). The thus obtained 5,6-dinitro-2-benzoimidazolone was refluxed in phosphorous oxychloride at 140° C. for 7 hours, followed by evaporating the excessive phosphorous oxychloride under reduced pressure, and neutralizing with an aqueous solution of sodium hydrogen carbonate, to thereby obtain yellow 5,6-dinitro-2-chlorobenzimidazole the 2-position of which was chloridized (yield 64.7%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338609B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-78624022d6884d3e9557c67970cc5689 |
| Source note | uspto-grants-2012_12 |