HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,5-Dimethyltetrazole → 1,1-Bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,5-Dimethyltetrazole | HCID 78825 | — |
| Edukt | 2,2'-Difluoro-4,4'-dimethylbenzophenone | HCID 14723981 | — |
| Edukt | Butyllithium | HCID 178418339 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 1,1-Bis(2-fluoro-4-methylphenyl)-2-(1-methyl-1H-tetrazol-5-yl)ethanol | HCID 14723992 | — |
Reaktionsbedingungen
| Temperatur | -10 °C |
|---|
Reaktionsschritte
To a solution of 1,5-dimethyltetrazole (4.6 g, 4.7 mmoles) in tetrahydrofuran (40 mL) at -=° C. was added butyl lithium solution (21.4 mL of a 2.2M solution, 4.7 mmoles). After stirring for 10 minutes, a solution of 2,2'-difluoro-4,4'-dimethylbenzophenone in tetrahydrofuran (15 mL) was added. The solution was stirred for 2.5 hours during which time it was allowed to warm to -10° C. The reaction was quenched by adding 1N hydrochloric acid. The layers were separated and the aqueous layer was extracted with methylene chloride. The combined organic fractions were dried (MgSO4) and evaporated. The residue was triturated with diethyl ether and crystallized from isopropyl acetate to give 8.0 g of the title compound; m.p.=150°-151° C. MS: M+ =344.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US04897490 |
| Quelldatensatz | uspto-grants-1990_01 |
| ORD ID | ord-3bbc23d6d833405b89f613091775c579 |
| Quellennotiz | uspto-grants-1990_01 |