HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1-(4-Methoxyphenyl)-1H-pyrazole
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | Hydroxyamine hydrochloride | HCID 443297 | — |
| Reactant | 1-[(4-methoxy)phenyl]-3-(ethoxycarbonyl)-1H-pyrazole | HCID 14372670 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 1-(4-Methoxyphenyl)-1H-pyrazole | HCID 12238131 | 69.9% |
Reaction Steps
To a solution of 1-[(4-methoxy)phenyl]-1H-pyrazole-5-[(4-(N-pyrrolidinocarbonyl)phenyl)carboxyamide-3-carboxylic acid (100 mg, 0.23 mmol) in 5 mL of acetonitrile was added triethylamine (0.064 mL, 0.46 mmol) and iso-butyl chloroformate (0.030 mL, 0.23 mmol). After stirring at ambient temperature for 30 min, there was added hydroxylamine hydrochloride (16 mg, 0.23 mmol). The reaction was stirred for 1 h and then the volatiles were removed. The residue was purified by prep HPLC (C18 reverse phase column, elution with a H2O/CH3CN gradient with 0.5% TFA) and lyophilized to afford 28 mg (27%) of the title compound as a white powder. LRMS (ES−): 562.1 (M−H+TFA)−.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06403620B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-707397dab7a94194bbe6c428dfab08fb |
| Source note | uspto-grants-2002_06 |