Bromine → 5-Bromo-2-(methylsulfanyl)pyrimidin-4(3H)-one

HRID 598081

Reaktionsgleichung

Reaktionsgleichung von HRID 598081
[CH3:1][S:2][C:3]1[NH:8][C:7](=[O:9])[CH:6]=[CH:5][N:4]=1.[Br:10]Br>C(O)(=O)C>[Br:10][C:6]1[C:7](=[O:9])[NH:8][C:3]([S:2][CH3:1])=[N:4][CH:5]=1

Komponenten

4

Edukt 2

HCID 24408BromineHCID 798232-(Methylthio)-1H-pyrimidin-4-one

Produkt 1

HCID 2405655-Bromo-2-(methylsulfanyl)pyrimidin-4(3H)-oneAusbeute 45,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel2×

Versuchsvorschrift

To a solution containing 2.0 g (14 mmol) of 2-(methylthio)pyrimidin-4(3H)-one in 10 ml of acetic acid under a nitrogen atmosphere was added 1.04 ml (14 mmol) of bromine in 2 ml acetic acid. The reaction was allowed to stir at room temperature for 30 min. The precipitated product was filtered, washed with acetic acid and suspended in hot acetic acid. To this suspension was added 0.2 ml bromine in 1 ml acetic acid. The product was collected, washed with acetic acid and recrystallized from ethanol to yield 1.4 g (45%) of product.

Aufarbeitung

  1. filtrationThe precipitated product was filtered
  2. washwashed with acetic acid
  3. additionTo this suspension was added 0.2 ml bromine in 1 ml acetic acid
  4. customThe product was collected
  5. washwashed with acetic acid
  6. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-b4e8dd88e8b74127887858907dba5968
Quelldatensatz
uspto-grants-2011_03
Patentnummer
US07897607B2

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