HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Acetic Acid → 2-(2,4-Difluorophenyl)-3-(1,2,4-triazol-1-yl)-2-(trimethylsilyloxy)propane
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Acetic Acid | HCID 176 | — |
| Edukt | 1-Trimethylsilyl-1,2,4-triazole | HCID 87558 | — |
| Edukt | 2-(2,4-Difluorophenyl)-2-methyloxirane | HCID 19708648 | — |
| Edukt | HCID 178507090 | HCID 178507090 | — |
| Lösungsmittel | Water | HCID 962 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 2-(2,4-Difluorophenyl)-3-(1,2,4-triazol-1-yl)-2-(trimethylsilyloxy)propane | HCID 15516903 | — |
Reaktionsschritte
5.13 g (0.03 moles) of 1,2-epoxy-2-(2,4-difluorophenyl)-propane are reacted with 6.35 g (0.045 moles) of 1-(trimethylsilyl)-1,2,4-triazole and 0.14 g (0.0015 moles) of 1,2,4-triazol-1-yl sodium in 40 ml of dimethyl formamide at 80° C. for 3 hours. Then the reaction mixture is cooled to room temperature, neutralized by glacial acetic acid, mixed with 200 ml of water and extracted twice with 50 ml of dichloromethane each. The combined extracts are washed three times with 50 ml of water each, dried over water-free sodium sulfate and evaporated in vacuo. After carrying out a separation as described in Example 5, removal of the solvent and crystallization from n-heptane 6.0 g (64.5%) of the title compound are obtained; m.p.: 51°-53° C.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05707976 |
| Quelldatensatz | uspto-grants-1998_01 |
| ORD ID | ord-f1cd7047a8394a479c696b57110fd9b6 |
| Quellennotiz | uspto-grants-1998_01 |