HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Lithium Hydroxide → 1-tert-Butyl-5-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Lithium Hydroxide | HCID 3939 | — |
| Edukt | Ethyl 1-(tert-butyl)-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate | HCID 2782985 | — |
| Lösungsmittel | Methanol--water (1/1) | HCID 22242641 | — |
| Produkt | 1-tert-Butyl-5-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid | HCID 1482039 | 92% |
Reaktionsschritte
To a stirred mixture of 1-tert-butyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (3.000 g; 11.4 mmol) in methanol/water (1:1 ratio, 50 mL) was added lithium hydroxide (0.383 g; 16.0 mmol) at room temperature. The mixture was heated to reflux for 2 hr, then allowed to cool to room temperature and concentrated to approximately half of the original volume. The resulting mixture was acidified with 1N HCl to ˜pH 1 and extracted with methylene chloride. The extracts were dried over sodium sulfate, filtered and concentrated to provide 1-tert-butyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid (2.47 g, 92%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07728029B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-74bbc7229e774ccda91f8e7165057b08 |
| Quellennotiz | uspto-grants-2010_06 |