HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → 4-Chloro-5,7-dimethyl-2-phenylimidazo[5,1-f][1,2,4]triazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 5,7-Dimethyl-2-phenylimidazo[5,1-f][1,2,4]triazin-4(3H)-one | HCID 135708002 | — |
| Product | 4-Chloro-5,7-dimethyl-2-phenylimidazo[5,1-f][1,2,4]triazine | HCID 58170015 | — |
Reaction Steps
700 mg (2.9 mmol) of 5,7-dimethyl-2-phenylimidazo[5,1-f][1,2,4]triazin-4(3H)-one (Example 15A) were dissolved in 8 ml of phosphoryl chloride and stirred at reflux for 12 h. The reaction mixture was poured into 170 ml of saturated sodium bicarbonate solution, and solid sodium bicarbonate was added until a pH of 7 had been reached. Ethyl acetate was added, and the mixture was extracted. The organic phase was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and concentrated on a rotary evaporator. This gave 657 mg (80% of theory) of the product as a solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09434731B2 |
| Source dataset | uspto-grants-2016_09 |
| ORD ID | ord-eee023c61ed747e2a328f887c5641585 |
| Source note | uspto-grants-2016_09 |