HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 68553228, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Cyanogen Bromide | HCID 10476 | — |
| Reactant | HCID 68549502 | HCID 68549502 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | Pentane | HCID 8003 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 68553228 | HCID 68553228 | — |
Reaction Steps
A mixture of 2.78 g (10.21 mmol) (2-aminobenzyl)(2,6-dimethoxybenzyl)amine and 1.5 g BrCN in 60 mL ethanol was heated at reflux for 10 hours. After evaporation, the resulting residue was dissolved in a small amount of dioxane, mixed with one equivalent 4N HCl in dioxane, the resulting solids were filtered out and dried. The resulting crude product was purified by MPLC (silica gel: Bischoff Prontoprep 60-2540-C18E, 32 μm; mobile phase: CH3CN/H2O+0.1% acetic acid), the resulting product was then dissolved in acetone and converted to the corresponding acetate by adding one equivalent of glacial acetic acid. Stirring the resulting solids [in] n-pentane and drying yielded 580 mg white solids.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08686002B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-3e0f1a670855455b8bf6401af7fe231f |
| Source note | uspto-grants-2014_04 |