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 | HCID 887 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Produkt | 1-tert-Butyl-5-(trifluoromethyl)-1H-pyrazole-4-carboxylic acid | HCID 1482039 | 80,3% |
Reaktionsschritte
To a solution of 1-tert-butyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (5 g, 21.2 mmol, purchased from Bionet) in CH3OH (45 mL) and water (45 mL) was added LiOH (0.54 g, 22.5 mmol). The reaction mixture was stirred at reflux for 4 h, and then the solution was concentrated under reduced pressure to remove the methanol. The residue was diluted with water and the solution was acidified to pH 2 with concentrated HCl. The resulting mixture was then extracted with ethyl acetate three times. The combined organic extracts were concentrated in vacuo to give 1-tert-butyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid (4.02 g, 80%), which was used without further purification.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07728029B2 |
| Quelldatensatz | uspto-grants-2010_06 |
| ORD ID | ord-7c97ea2069d945458aadd4baa1d276b4 |
| Quellennotiz | uspto-grants-2010_06 |