HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Hydrogen Bromide → 1-Phenyl-2-(pyridin-3-yl)ethan-1,2-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Hydrogen Bromide | HCID 260 | — |
| Edukt | Water | HCID 962 | — |
| Edukt | Benzyl-(3-pyridyl)-ketone-hydrochloride | HCID 21558184 | — |
| Lösungsmittel | Dimethyl Sulfoxide | HCID 679 | — |
| Produkt | 1-Phenyl-2-(pyridin-3-yl)ethan-1,2-dione | HCID 10987556 | — |
Reaktionsschritte
23.4 g (0.1 mol) of benzyl-(3-pyridyl)-ketone-hydrochloride are taken up in 180 ml of dimethyl sulphoxide and the solution is treated with 20 ml of 48% hydrobromic acid. The reaction mixture is stirred for 18 hours at 80° - 85°C and subsequently poured on a mixture of 800 g of ice and 1000 ml of water. The yellow emulsion is extracted with 2 × 200 ml of ethyl acetate. The two organic phases are combined, washed with water and dried over sodium sulphate. The red solution is concentrated in a rotary evaporator until a residual oil is left which is distilled in a bulb tube at 140° - 150°C/0.1 Torr (m.p. 56° - 57°C).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US03940486 |
| Quelldatensatz | uspto-grants-1976_02 |
| ORD ID | ord-e45a5ce9e6f745799c42c59104dfb605 |
| Quellennotiz | uspto-grants-1976_02 |