HuagongsheHuagongshe Chemistry Print Report · For research reference only
1H-1,2,4-Triazole → HCID 59208302, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1H-1,2,4-Triazole | HCID 9257 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1,4-Dibenzyl-2-(chloromethyl)piperazine | HCID 10663119 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 59208302 | HCID 59208302 | 99.7% |
Reaction Steps
To a solution of 1,2,4-triazole (48.3 mg, 0.70 mmol) in DMF (2 ml) was added NaH (18.3 mg, 0.76 mmol). After 10 minutes stirring, 1,4-dibenzyl-2-(chloromethyl)piperazine (200 mg, 0.64 mmol) and KI (156 mg, 0.70 mmol) were added to the mixture. The mixture was stirred at 60° C. overnight. The mixture was diluted with EtOAc and washed with water and brine. The organic layer was dried over MgSO4, filtered and concentrated in vacuo. The resulting residue was purified by column chromatography on NH-silica gel (Hex/AcOEt=¼) to give 1,4-dibenzyl-2-(1H-1,2,4-triazol-1-ylmethyl)piperazine (220.0 mg, 99.7%): HPLC-MS (ESI): Calcd for C21H25N5 [M+H]+ 348, found: 348.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07674797B2 |
| Source dataset | uspto-grants-2010_03 |
| ORD ID | ord-a7ebc2f531b34e399c79877c20b2c85e |
| Source note | uspto-grants-2010_03 |