HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzene → HCID 178523136, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | Hydrazinecarboxaldehyde | HCID 12229 | — |
| Reactant | HCID 58597276 | HCID 58597276 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 178523136 | HCID 178523136 | — |
Reaction Steps
(N-(4-cyanophenethyl)-2,2,2-trifluoroacetamide (0.61 g, 2.52 mmol) was azeotroped with benzene and was dissolved in 10 mL of anhydrous EtOH. To this solution dry HCl was bubbled though for 90 min at 0 C. The solvent was evaporated to dryness under high vacuum to give a yellow solid. This yellow solid and formohydrazide (151 mg, 2.52 mmol) was dissolved in 10 mL of dry pyridine and the resulting solution was refluxed for 2 h. After cooling to RT, pyridine was evaporated and the residue was treated with 5% HCl, extracted with EtOAc, dried over Na2SO4, filtered, and evaporated to dryness. Flash chomatography (SiO2, EtOAc/DCM=1:1 to Dcm/MeOH=10:1) afforded N-(4-(4H-1,2,4-triazol-3-yl)phenethyl)-2,2,2-trifluoroacetamide as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07662811B2 |
| Source dataset | uspto-grants-2010_02 |
| ORD ID | ord-268104e373a24803a8718b5123111943 |
| Source note | uspto-grants-2010_02 |