HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Trifluoroacetic acid → 5-Cyano-3-methylpyridine-2-carboxylic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Trifluoroacetic acid | HCID 6422 | — |
| Edukt | 1,3-Dimethoxybenzene | HCID 9025 | — |
| Edukt | 5-Cyano-3-methyl-pyridine-2-carboxylic acid tert-butyl ester | HCID 66665826 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 5-Cyano-3-methylpyridine-2-carboxylic acid | HCID 66665846 | — |
Reaktionsschritte
To a solution of 8.50 g (38.9 mmol) 5-cyano-3-methyl-pyridine-2-carboxylic acid tert-butyl ester in 51 ml (389 mmol) 1,3-dimethoxybenzene were added 85 ml TFA and stirred for 6.5 h. The reaction mixture was diluted with toluene and evaporated. The residue was taken up in toluene and evaporated (2×). The product was crystallized from TBME/hexanes to give the title compound as a white powder. HPLC: RtH1=2.314 min; ESIMS [M+Na]+=163; 1H-NMR (360 MHz, CDCl3): δ 8.77 (s, 1H), 8.07 (s, 1H), 2.87 (s, 3H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08524897B2 |
| Quelldatensatz | uspto-grants-2013_09 |
| ORD ID | ord-d190e2cba5834572b06ba6de8bb7dcc5 |
| Quellennotiz | uspto-grants-2013_09 |