HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrochloric Acid → 2-Methyl-6-(trifluoromethyl)nicotinic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrochloric Acid | HCID 313 | — |
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Lithium hydroxide, monohydrate | HCID 168937 | — |
| Edukt | Methyl 2-methyl-6-(trifluoromethyl)nicotinate | HCID 2779428 | — |
| Lösungsmittel | Methanol--water (1/1) | HCID 22242641 | — |
| Produkt | 2-Methyl-6-(trifluoromethyl)nicotinic acid | HCID 2775683 | 90,9% |
Reaktionsschritte
6.68 g (0.0305 mol) of 2-methyl-6-trifluoromethyl-nicotinic acid methyl ester (prepared in the manner described in Heterocycles, 46, 129 (1997)) are dissolved in 250 ml of methanol/water (3:1 mixture) and 1.92 g (0.046 mol) of lithium hydroxide hydrate are added in portions at 22° C. After 4 hours at 22° C., the reaction mixture is added to ethyl acetate and 2N hydrochloric acid; the organic phase is washed three times with water, dried with sodium sulfate and concentrated by evaporation, and the residue is triturated with a small amount of hexane. After filtering, 5.69 g (90% of theory) of the expected 2-methyl-6-trifluoromethyl-nicotinic acid having a melting point of 147-149° C. are obtained.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06890885B2 |
| Quelldatensatz | uspto-grants-2005_05 |
| ORD ID | ord-6786c08f58184e3793d5a6323c3caed0 |
| Quellennotiz | uspto-grants-2005_05 |