HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 4-Bromo-1-{3-fluoro-4-[(phenylmethyl)oxy]phenyl}-6-methyl-1h-indazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 4-Benzyloxy-3-fluorophenylboronic Acid | HCID 2737788 | — |
| Reactant | 4-Bromo-6-methyl-1H-indazole | HCID 24728801 | — |
| Catalyst | Cupric acetate | HCID 8895 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-Bromo-1-{3-fluoro-4-[(phenylmethyl)oxy]phenyl}-6-methyl-1h-indazole | HCID 59272966 | 107% |
Reaction Steps
The 4-bromo-6-methyl-1H-indazole (950 mg, 4.5 mmol), the {3-fluoro-4-[(phenylmethyl)oxy]phenyl}boronic acid (2.2 g, 9 mmol), copper (II) acetate (1.22 g, 6.75 mmol) and pyridine (0.73 mL, 9 mmol) in DCM (80 mL) were stirred in the presence of molecular sieves (4 A, 2 g) in air. After 40 hours the mixture was filtered through a pad of celite and concentrated to afford 3.3 g of crude material. This was purified by flash chromatography (Biotage SP4, 40+M silica column) with a gradient of EtOAc 0 to 30% in hexane to afford 1.98 g of desired compound (D12) slightly impure but carried forward.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07960563B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-29910b39b6f74713843098eeb127efd8 |
| Source note | uspto-grants-2011_06 |