HuagongsheHuagongshe Chemistry Print Report · For research reference only
p-Toluenesulfonic acid → HCID 178499497, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | p-Toluenesulfonic acid | HCID 6101 | — |
| Reactant | Dimethyl acetylsuccinate | HCID 112039 | — |
| Reactant | 5-([1,1'-biphenyl]-3-yl)-3H-1,2,4-triazol-3-amine | HCID 86695072 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 178499497 | HCID 178499497 | — |
Reaction Steps
In a 100 ml RBF, equipped with a Dean-Stark trap (filled with molecular sieves), was added 5-([1,1′-biphenyl]-3-yl)-3H-1,2,4-triazol-3-amine (1.133 g, 4.80 mmol), dimethyl 2-acetylsuccinate (2.334 mL, 14.39 mmol) followed by Xylene (50 mL) and Ts-OH (9.12 mg, 0.048 mmol). The reaction was heated at reflux for 5 hrs. Filtered and washed by hexanes to collect the off-white solid, which was used directly for the next step. 1H-NMR (500 MHz, CDCl3) δ 2.26 (3H, s), 3.65 (2H, s), 3.72 (3H, s), 7.35-7.36 (1H, m), 7.44-7.46 (2H, m), 7.47-7.48 (1H, m), 7.64-7.66 (2H, m), 7.73-7.75 (1H, m), 8.13-8.15 (1H, m), 8.43 (1 H, s).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09034882B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-34a6a127ef8646f4b597541a9a1a9507 |
| Source note | uspto-grants-2015_05 |