Acetone → 1-(4,6-Dimethoxypyrimidin-2-yl)propan-2-one

HRID 916732

Reaktionsgleichung

Reaktionsgleichung von HRID 916732
[H-].[Na+].C1COCC1.[CH3:8][O:9][C:10]1[CH:15]=[C:14]([O:16][CH3:17])[N:13]=[C:12](S(C)(=O)=O)[N:11]=1.[CH3:22][C:23]([CH3:25])=[O:24]>O>[CH3:8][O:9][C:10]1[CH:15]=[C:14]([O:16][CH3:17])[N:13]=[C:12]([CH2:22][C:23](=[O:24])[CH3:25])[N:11]=1

Komponenten

6

Edukt 4

HCID 180AcetoneHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 8383634,6-Dimethoxy-2-(methylsulfonyl)pyrimidine

Produkt 1

HCID 112640521-(4,6-Dimethoxypyrimidin-2-yl)propan-2-oneAusbeute 22,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
30 °C

Versuchsvorschrift

In a reactor were placed 16.0 g (0.4 moles) of 60% sodium hydride, 400 ml of THF and 43.6 g (0.2 moles) of 4,6-dimethoxy-2-methanesulfonylpyrimidine. The reactor contents were heated to 30° C. Thereto was dropwise added 39.4 g (0.68 moles) of acetone, followed by a reaction for 2 hours. After the completion of the reaction, 350 ml of water was added and extraction with 500 ml of ethyl acetate was conducted. The ethyl acetate layer was concentrated. The concentrate was subjected to distillation under reduced pressure to obtain 8.8 g (44.9 m moles) of 1-(4,6-dimethoxypyrimidine-2-yl)-2-propanone. Refractive index n20D: 1.5181

Aufarbeitung

  1. customIn a reactor were placed
  2. customfollowed by a reaction for 2 hours
  3. additionwas added
  4. extractionextraction with 500 ml of ethyl acetate
  5. concentrationThe ethyl acetate layer was concentrated
  6. distillationThe concentrate was subjected to distillation under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-9d935eb6d0fd4a299d9ebf267e4321da
Quelldatensatz
uspto-grants-2007_09
Patentnummer
US07271263B2

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