2-Bromopropiophenone → 2-Amino-4-phenyl-5-methylthiazole

HRID 1009043

Reaktionsgleichung

Reaktionsgleichung von HRID 1009043
Br[CH:2]([CH3:11])[C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=O.[NH2:12][C:13]([NH2:15])=[S:14]>C(O)C>[CH3:11][C:2]1[S:14][C:13]([NH2:15])=[N:12][C:3]=1[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

Komponenten

4

Edukt 2

HCID 164522-BromopropiophenoneHCID 2723790Thiourea

Produkt 1

HCID 961292-Amino-4-phenyl-5-methylthiazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
57.5 °C

Versuchsvorschrift

To a solution of 2-bromo-1-phenyl-propan-1-one (3.64 g, 17.1 mmol) in 30 mL of ethanol was added thiourea (1.30 g, 1.00 eq.) and the mixture vigorously stirred at 55-60° C. for 4 h. Pouring onto crashed ice/Na2CO3, twofold extraction with ethyl acetate, washing with water and brine, drying over sodium sulfate, and evaporation of the solvents, followed by crystallization from ethyl acetate/hexane, left 2.87 g of the title product as off-white crystals.

Aufarbeitung

  1. additionPouring
  2. extractionice/Na2CO3, twofold extraction with ethyl acetate
  3. washwashing with water and brine
  4. dry with materialdrying over sodium sulfate, and evaporation of the solvents
  5. customfollowed by crystallization from ethyl acetate/hexane
  6. waitleft 2.87 g of the title product as off-white crystals

Quellen und Nachweise

ORD-Eintrag
ord-1d3dad42707b41e2912134afaf88456d
Quelldatensatz
uspto-grants-2011_07
Patentnummer
US07973051B2

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