HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → 5-(3-chloro-benzylamino)-2-methyl-2H-pyrazole-3-carboxylic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | 3-Chlorobenzaldehyde | HCID 11477 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | methyl 3-amino-1-methyl-1H-pyrazole-5-carboxylate | HCID 13248993 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 5-(3-chloro-benzylamino)-2-methyl-2H-pyrazole-3-carboxylic acid methyl ester | HCID 57619417 | — |
Reaction Steps
5-Amino-2-methyl-2H-pyrazole-3-carboxylic acid methyl ester (644, 1.3 g, 8.0 mmol) was combined with 3-chlorobenzaldehyde (645, 0.95 mL, 8.4 mmol) and acetonitrile (40 mL). Trifluoroacetic acid (3.2 mL, 42.0 mmol) was added followed by triethylsilane (6.7 mL, 42.0 mmol). The reaction was heated to reflux overnight and then concentrated. Ethyl acetate was added and the solution was washed with 1N potassium carbonate. The organic portion was dried over anhydrous sodium sulfate, filtered and concentrated. The compound (646, 0.944 g, 42%) was crystallized from a mixture of ethyl acetate:hexane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09169250B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-077a9a575b4749f693d3e77c59977f9b |
| Source note | uspto-grants-2015_10 |