HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86601246, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethylenediamine | HCID 3301 | — |
| Reactant | Trimethylaluminum | HCID 16682925 | — |
| Reactant | HCID 86601247 | HCID 86601247 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | HCID 86601246 | HCID 86601246 | 19% |
Reaction Steps
To a solution of Me3Al (1.36 mL, 2M soln in toluene) at 0° C. under N2, add ethylenediamine (185 μL, 0.36 mmol) and stir for several minutes warming to RT. Add 1-(3,5-bis-trifluoromethyl-benzyl)-5-phenyl-1H-[1,2,3]triazole-4-carboxylic acid methyl ester (750 mg, 1.69 mmol) dissolved in toluene to this solution. Reflux reaction for 3.5 hours at 110° C. Cool to RT and stir for 12 hours. Quench reaction with MeOH (2 mL), add H2O (2 mL) and extract with CH2Cl2 (4 mL×2). Dry over Na2SO4 and concentrate to afford title compound (30 mg, 4%). MS (IS) 440.1 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07320994B2 |
| Source dataset | uspto-grants-2008_01 |
| ORD ID | ord-7486854bc5b543db95f639e001bcac80 |
| Source note | uspto-grants-2008_01 |