Reaktionsgleichung
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=O.[NH2:11][C:12]([NH2:14])=[S:13].O>CO>[NH2:14][C:12]1[S:13][CH:2]=[C:3]([C:5]2[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=2)[N:11]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
A solution of 19.9 g (0.10 mol) of α-bromo-acetophenone and 11.4 g (0.15 mol) of thiourea in 75 ml of methanol is refluxed for 2 h. It is evaporated to dryness under reduced pressure and the evaporation residue is taken up with water. The resulting solution, heated to the reflux temperature, is treated with CXA charcoal and then rendered alkaline with aqueous ammonia. The precipitate formed is isolated by filtration and purified by recrystallization from isopropanol, with CXA charcoal treatment. to give 15 g (yield: 85.15%) of the expected product in the form of water-insoluble white needles. M.p. (inst.)=150° C.
Aufarbeitung
- customIt is evaporated to dryness under reduced pressure
- temperatureThe resulting solution, heated to the reflux temperature
- additionis treated with CXA charcoal
- customThe precipitate formed
- customis isolated by filtration
- custompurified by recrystallization from isopropanol, with CXA charcoal treatment
Quellen und Nachweise
- ORD-Eintrag
- ord-c7e2722c24ed4f17a5955e331ecbdc30
- Quelldatensatz
- uspto-grants-1989_07
- Patentnummer
- US04847274
Verknüpfte Notizen
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