HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl acetylsuccinate → HCID 178499519, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl acetylsuccinate | HCID 112039 | — |
| Reactant | 3-Amino-5-phenylpyrazole | HCID 136655 | — |
| Catalyst | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | HCID 178499519 | HCID 178499519 | 86% |
Reaction Steps
To a solution of 3-phenyl-1H-pyrazol-5-amine (4 g, 25.1 mmol) and dimethyl 2-acetylsuccinate (12 mL, 74.0 mmol) in xylene (120 mL) was added p-toluenesulfonic acid monohydrate (50 mg, 0.263 mmol). The reaction mixture was heated at reflux under a Dean-Stark trap for 20 h. The solid was filtered and washed with hexanes to afford the title compound (6.4 g, 86%). 1H-NMR (400 MHz, MeOD) δ ppm 2.37 (3H, s), 3.66 (2H, s), 3.72 (3H, s), 6.46 (1H, s), 7.34-7.53 (3H, m), 7.87-8.06 (2H, m).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08633200B2 |
| Source dataset | uspto-grants-2014_01 |
| ORD ID | ord-4d883600fa2a4fe3a7faa7cd0d16926f |
| Source note | uspto-grants-2014_01 |