HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → 1-(5-Methyl-4-phenyl-4H-1,2,4-triazol-3-yl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Piperazine | HCID 4837 | — |
| Reactant | HCID 12217059 | HCID 12217059 | — |
| Solvent | Dichloromethane methanol | HCID 21226129 | — |
| Product | 1-(5-Methyl-4-phenyl-4H-1,2,4-triazol-3-yl)piperazine | HCID 22418762 | — |
Reaction Steps
A mixture of 3-bromo-5-methyl-4-phenyl-4H-1,2,4-triazole (4.16 g), 15.07 g of piperazine and 20 ml of pyridine is stirred at 100° under nitrogen for 22 h. The reaction is monitored by TLC (8% methanol/methylene chloride) and after this period of time no change occurs. The mixture is subsequently placed in a Parr bomb and heated in an oil bath at 180° for 24 h. Bomb pressure increases by 40 psi. The mixture is worked up by partitioning between chloroform and water. The organic phase is washed with saturated aqueous sodium bicarbonate (2×) and with saline (2×), dried over sodium sulfate and concentrated to a solid, the product is recrystallized in ethyl acetate, MS [M+H]+ 243.1484
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05120843 |
| Source dataset | uspto-grants-1992_06 |
| ORD ID | ord-2b83b1e9e4414bfeb8a748b76fe69321 |
| Source note | uspto-grants-1992_06 |