HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isobutyryl chloride → 6-Bromo-3-(propan-2-yl)[1,2,4]triazolo[4,3-a]pyridine--hydrogen chloride (1/1)
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isobutyryl chloride | HCID 62325 | — |
| Reactant | 5-Bromo-2-hydrazinopyridine | HCID 11535699 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | 6-Bromo-3-(propan-2-yl)[1,2,4]triazolo[4,3-a]pyridine--hydrogen chloride (1/1) | HCID 22170177 | — |
Reaction Steps
A 500 ml three-necked round-bottomed flask equipped with a mechanical stirrer and a condenser, connected on top to a nitrogen bubbler and a thermometer, was charged with 5-bromo-pyridin-2-yl-hydrazine (43.4 g, 0.231 moles) and isobutyryl chloride (218 ml, 2.08 moles). The mixture was gently refluxed for 3 hours. The heating source was then replaced with an ice-water bath and the slurry cooled to room temperature. Hexane (220 ml) was added and the slurry stirred at room temperature for 15 minutes and filtered. The cake was washed with hexane (3×70 ml) and then dried in a vacuum-oven (35° C.) for 48 hours. The title compound was obtained as an off-white powder (58.96 g, yield 92.3%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07005523B2 |
| Source dataset | uspto-grants-2006_02 |
| ORD ID | ord-5670a85f1f5a475c829c77a7072638ae |
| Source note | uspto-grants-2006_02 |