HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → HCID 178422299, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Ethyl 2-bromo-3-oxobutanoate | HCID 11206579 | — |
| Reactant | HCID 178418690 | HCID 178418690 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 178422299 | HCID 178422299 | 78.1% |
Reaction Steps
A mixture of 3-methyl-1H-pyrazol-5-amine (0.186 g, 1.92 mmol) and acetic acid (3.71 mL, 65.2 mmol) was slightly heated until complete dissolution and the resultant solution was cooled to RT and mixed with ethyl 2-bromo-3-oxobutanoate (1.20 g, 5.74 mmol). The resultant reaction mixture was stirred at RT for 16 h, after which time the reaction mixture was diluted with diethyl ether, cooled to 0° C. and stirred at that temperature for 30 min. The white solid precipitate was separated by filtration and washed with cold diethyl ether and dried to give the desired product (363 mg, 78%) as a white solid. LCMS calculated for C8H9BrN3O (M+H)+: m/z=242.0, 244.0. found: 241.9, 244.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09399640B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-b09f5e393afb4ac58d2a499dfc9d06d5 |
| Source note | uspto-grants-2016_07 |