Potassium Hydroxide → HCID 178516654, Verbindung

HRID 424676

Reaktionsgleichung

Reaktionsgleichung von HRID 424676
[OH-].[K+].[SH:3][C:4]1[N:9]=[C:8]([OH:10])[CH:7]=[C:6]([OH:11])[N:5]=1.[F:12][C:13]1[C:20]([F:21])=[CH:19][CH:18]=[CH:17][C:14]=1[CH2:15]Br>CN(C=O)C.O.C1COCC1>[F:12][C:13]1[C:20]([F:21])=[CH:19][CH:18]=[CH:17][C:14]=1[CH2:15][S:3][C:4]1[N:9]=[C:8]([OH:10])[CH:7]=[C:6]([OH:11])[N:5]=1

Komponenten

7

Edukt 3

HCID 14797Potassium HydroxideHCID 5179841-(Bromomethyl)-2,3-difluoro-benzeneHCID 178516656HCID 178516656, Verbindung

Produkt 1

HCID 178516654HCID 178516654, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A solution of potassium hydroxide (5.67 g) was added dropwise to a suspension of 2-mercaptopyrimidine-4,6-diol (14.56 g) in DMF (78 ml) and H2O (39 ml) and the mixture stirred for 30 min. A solution of 2,3-difluorobenzyl bromide (20.86 g) in THF (16 ml) was then added dropwise and the mixture stirred for 18 h. The reaction was then cooled to 0° C. and the precipitate was filtered and washed with H2O (4×100 ml) before drying in vacuo to afford the subtitle compound as a cream solid. Yield: 22.4 g.

Aufarbeitung

  1. stirringthe mixture stirred for 18 h
  2. filtrationthe precipitate was filtered
  3. washwashed with H2O (4×100 ml)
  4. custombefore drying in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-8db37646f9a14f1eb8e527663de246fa
Quelldatensatz
uspto-grants-2012_01
Patentnummer
US08106063B2

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