HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 9-[1-(2,2,2-Trichloroethoxycarbonyl)-4-piperidylidene]xanthene
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Sodium Hydroxide | HCID 14798 | — |
| Edukt | 2,2,2-Trichloroethyl chloroformate | HCID 87063 | — |
| Edukt | 1-Methyl-4-xanthen-9-ylidene-piperidine | HCID 10039173 | — |
| Lösungsmittel | Toluene | HCID 1140 | — |
| Produkt | 9-[1-(2,2,2-Trichloroethoxycarbonyl)-4-piperidylidene]xanthene | HCID 15289478 | — |
Reaktionsschritte
To a mixture of 430 mg (1.55 mmol) of 1-methyl-4-(9H-xanthene-9-ylidene)piperidine [Tetrahedron Letters, 29, 5701 (1988)] and 649 μL (4.65 mmol) of triethylamine in 20 mL of dry toluene at 85° C. under an atmosphere of argon was added over 10 min 1.06 mL (7.7 mmol) of 2,2,2-trichloroethyloxycarbonyl chloride. After 30 min the mixture was cooled to room temperature, poured into a solution of 25% aqueous sodium hydroxide, and was extracted with ethyl acetate (3×). The combined organic portions were dried over sodium sulfate, filtered, and concentrated with vacuo to afford the title compound as a crude oil.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US05416087 |
| Quelldatensatz | uspto-grants-1995_05 |
| ORD ID | ord-56a04910b677402a8876a4b78d2c3b06 |
| Quellennotiz | uspto-grants-1995_05 |