HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cesium carbonate → HCID 69939744, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | Methyl 4-bromo-2-(bromomethyl)benzoate | HCID 22031079 | — |
| Reactant | 5-(4-Chlorophenyl)-4-(3,3,3-trifluoro-2-hydroxypropyl)-2,4-dihydro-3H-1,2,4-triazol-3-one | HCID 58460118 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 69939744 | HCID 69939744 | — |
Reaction Steps
450 mg (1.30 mmol) of the compound from Example 4A and 715 mg (2.19 mmol) of cesium carbonate were suspended in 6 ml of acetonitrile, and 708 mg (1.61 mmol) of methyl 4-bromo-2-(bromomethyl)benzoate were added. The mixture was stirred under reflux for 20 h. The precipitated solid was filtered off and the filtrate was concentrated under reduced pressure to a volume of about 1.5 ml. After addition of 1 ml of 1 N hydrochloric acid, the mixture was directly purified chromatographically [Method 19]. This gave 545 mg (64% of theory) of the target compound in a purity of 92%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09187466B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-95cc1da75d7341809dda5c707f839e7c |
| Source note | uspto-grants-2015_11 |