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3-Chloro-2,4-pentanedione → HCID 9344223, Verbindung

HRID 1498946
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1498946
[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:3]=1[C:4]([NH2:6])=[S:5].Cl[CH:13]([C:17](=O)[CH3:18])[C:14](=[O:16])[CH3:15]>C(O)C>[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[CH:8]=[CH:7][C:3]=1[C:4]1[S:5][C:13]([C:14](=[O:16])[CH3:15])=[C:17]([CH3:18])[N:6]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 743283-Chloro-2,4-pentanedioneHCID 25176802,4-Dimethylbenzenecarbothioamide

Produkt 1

HCID 9344223HCID 9344223, VerbindungAusbeute 37 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

To ethanol (20 ml), 2,4-dimethylthiobenzamide (2.00 g) and 3-chloropentane-2,4-dione (1.79 g) were added, and the mixture was stirred under heat reflux for 4 hours. After the mixture was allowed to cool to a room temperature, from the mixture ethanol was distilled off under a reduced pressure. To the resulting residue, ethyl acetate was added, and the mixture was heated and stirred. After the mixture was allowed to cool to a room temperature, the precipitate was separated by filtration, washed with ethyl acetate, and then dried under a reduced pressure to give the title compound (1.10 g, 37%).

Aufarbeitung

  1. temperatureunder heat
  2. temperaturereflux for 4 hours
  3. distillationwas distilled off under a reduced pressure
  4. additionTo the resulting residue, ethyl acetate was added
  5. temperaturethe mixture was heated
  6. stirringstirred
  7. customthe precipitate was separated by filtration
  8. washwashed with ethyl acetate
  9. customdried under a reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-532f438747f44bc58a01e1341693363c
Quelldatensatz
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09200008B2

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