HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 67407291, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 4-Bromo-2-(bromomethyl)-1-fluorobenzene | HCID 13553295 | — |
| Reactant | 3-(4-Chlorophenyl)-4-cyclopropyl-1H-1,2,4-triazol-5(4H)-one | HCID 58012199 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 67407291 | HCID 67407291 | — |
Reaction Steps
300 mg (1.27 mmol) of 5-(4-chlorophenyl)-4-cyclopropyl-2,4-dihydro-3H-1,2,4-triazol-3-one [preparation according to WO 2007/134862 Example 36A] and 622 mg (1.91 mmol) of cesium carbonate were suspended in 5 ml of acetonitrile, and 536 mg (1.40 mmol) of 4-bromo-2-(bromomethyl)-1-fluorobenzene were added. The mixture was stirred under reflux for 18 h. The precipitated solid was then filtered off and the filtrate was concentrated under reduced pressure to a volume of about 1.5 ml. After addition of 0.5 ml of 1 N hydrochloric acid, the mixture was directly purified chromatographically [Method 19]. This gave 427 mg (56% of theory) of the target compound in a purity of 71%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09187466B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-951dc5b393e54e889a10e4fdad19f7d9 |
| Source note | uspto-grants-2015_11 |