Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Iodine | HCID 807 | — |
| Reactant | Thiourea | HCID 2723790 | — |
| Reactant | HCID 59323905 | HCID 59323905 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59323904 | HCID 59323904 | — |
Reaction Steps
A solution of 1-(4-pyrazol-1-yl-phenyl)-propan-2-one (6.9 g, 34.46 mmol) in pyridine (30 ml) is treated with thiourea (2.6 g, 34.46 mmol) followed by iodine (8.7 g, 34.46 mmol) and heated to 80° C. After 8 hours, the reaction mixture is allowed to cool to room temperature and the resulting suspension is filtered and washed with EtOAc. The filtrate is concentrated in vacuo to afford an oil. The oil is dissolved in EtOAc (200 ml) and washed with NaHCO3 (2×100 ml), brine (100 ml), dried (MgSO4) and concentrated in vacuo to afford a sticky solid. EtOH is added to the crude residue and the resulting precipitate is filtered and dried to afford the title compound (MH+ 257.29).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07799810B2 |
|---|
| Source dataset | uspto-grants-2010_09 |
|---|
| ORD ID | ord-b982f91176cb4129ab3a0e047ad57e80 |
|---|
| Source note | uspto-grants-2010_09 |
|---|