HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trichloroacetyl chloride → 2,9-Dimethyl-3-trichloroacetylimidazo[1,2-a]benzimidazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trichloroacetyl chloride | HCID 6420 | — |
| Reactant | 2,4-Dimethylimidazo[1,2-a]benzimidazole | HCID 828269 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | 2,9-Dimethyl-3-trichloroacetylimidazo[1,2-a]benzimidazole | HCID 19040812 | — |
Reaction Steps
Pour 5.45 g (30 mmol) of freshly distilled trichloroacetyl chloride dropwise into a boiling solution of 2,9-dimethylimidazo[1,2-a]benzimidazole (3.7 g; 20 mmol)--obtained as described in Khim. Geterotsikl Soedin, 86, (7), 918-925--in 50 ml of xylene, with vigorous stirring, over a period of 20 to 30 minutes. The mixture is then heated at reflux for two hours until the product which has initially precipitated is completely dissolved. Cool and filter. Concentrate the mother liquors and add petroleum ether. Combine with the precipitate obtained earlier and repeat the operation. The combined precipitates are treated with an aqueous solution of sodium hydrogen carbonate and then recrystallised from ethyl acetate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05623073 |
| Source dataset | uspto-grants-1997_04 |
| ORD ID | ord-61de2979af5447788006ba4dcceb3672 |
| Source note | uspto-grants-1997_04 |