HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 2-bromo-4-(1-(4-methoxybenzyl)-1H-1,2,3-triazol-4-yl)pyridine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 1-(Azidomethyl)-4-methoxybenzene | HCID 10931767 | — |
| Reactant | 2-Bromo-4-ethynylpyridine | HCID 23436810 | — |
| Reactant | Sodium Ascorbate | HCID 23667548 | — |
| Catalyst | Copper sulfate pentahydrate | HCID 24463 | — |
| Solvent | tert-Butanol | HCID 6386 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | 2-bromo-4-(1-(4-methoxybenzyl)-1H-1,2,3-triazol-4-yl)pyridine | HCID 86680800 | 77% |
Reaction Steps
To a flask containing 2-bromo-4-ethynylpyridine (1 g, 5.49 mmol) was added 4-methoxybenzyl azide (896 mg, 5.49 mmol), CuSO4(H2O)5 (137 mg, 0.549 mmol), sodium ascorbate (544 mg, 2.75 mmol), water (13.7 mL) and tBuOH (13.7 mL) and the reaction was stirred for 16 h at rt. The reaction was diluted with EtOAc (50 mL) and washed with saturated aqueous NaHCO3 (1×20 mL) and brine (1×20 mL). The organic phase was dried (MgSO4), filtered, and purified by silica gel chromatography using a gradient solvent system of 30-70% EtOAc/Hexanes. Concentration of the product fractions yielded 2-bromo-4-(1-(4-methoxybenzyl)-1H-1,2,3-triazol-4-yl)pyridine (1.46 g, 77%) as a white powder. MS ESI calcd for C15H13BrN4O [M+H]+ 345, found 345.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08796310B2 |
| Source dataset | uspto-grants-2014_08 |
| ORD ID | ord-0541a742e24e42b4876e9b0f0320e7ee |
| Source note | uspto-grants-2014_08 |