HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
2-Methyl-2-butene → 2-(Butyl-ethyl-amino)-5-trifluoromethyl-benzoic acid
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 2-Methyl-2-butene | HCID 10553 | — |
| Edukt | Sodium Chlorite | HCID 23668197 | — |
| Edukt | Sodium Phosphate, Monobasic, Dihydrate | HCID 23673460 | — |
| Edukt | 2-(Butyl-ethyl-amino)-5-trifluoromethyl-benzaldehyde | HCID 86626752 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | tert-Butanol | HCID 6386 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | 2-(Butyl-ethyl-amino)-5-trifluoromethyl-benzoic acid | HCID 63513446 | 0,1% |
Reaktionsschritte
2-(Butyl-ethyl-amino)-5-trifluoromethyl-benzaldehyde (1.72 g) is dissolved in a mixed solvent of tert-butanol (8 ml) and water (2 ml), and thereto are added 2-methyl-2-butene (4 ml), sodium dihydrogenphosphate dihydrate (1.37 g) and sodium chlorite (1.82 g) under ice-cooling, and the mixture is stirred for 2 hours. Thereto are added ethyl acetate and a 1N-hydrochloric acid and the mixture is separated, and the organic layer is washed with a saturated brine, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting residue is purified by silica gel column chromatography (chloroform:methanol=1:0→9:1) to give 2-(butyl-ethyl-amino)-5-trifluoromethyl-benzoic acid (1.29 mg). MS (m/z): 290 [M+H]+
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07906517B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-b05c036477c34a1f937854c866af659a |
| Quellennotiz | uspto-grants-2011_03 |