HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 67384969, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | 3-Methyl-4-phenylpyrazol | HCID 139601 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 67384969 | HCID 67384969 | 62.3% |
Reaction Steps
To a solution of 5-methyl-4-phenyl-1H-pyrazole (3.0 g, 18.96 mmol) in acetic acid (glacial, 100 mL) was added bromine (1.457 mL, 28.4 mmol) at room temperature. The reaction was stirred at room temperature for 2 h. After quenched with aqueous solution of Na2SO3 (10% wt aq., 10 mL), the reaction was concentrated and extracted with EtOAc, washed with brine, dried over MgSO4, and purified by silica gel column chromatography to give the title compound as yellow oil (2.8 g). LCMS m/z=236.9 [M+H]+; 1H NMR (400 MHz, DMSO-d6) δ ppm 2.26 (s, 3H), 7.24-7.54 (m, 5H), 13.13 (s, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09012478B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-8909991298544bfa8e02032afb069846 |
| Source note | uspto-grants-2015_04 |