Water → HCID 46836756, Verbindung

HRID 474222Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 474222
Cl[CH2:2][CH:3]([OH:6])[CH2:4][OH:5].C(=O)([O-])[O-].[Cs+].[Cs+].[OH:13][C:14]1[CH:15]=[N:16][C:17]([C:20]2[CH:21]=[C:22]([CH:37]=[CH:38][CH:39]=2)[CH2:23][N:24]2[C:29](=[O:30])[CH:28]=[CH:27][C:26]([C:31]3[CH:32]=[N:33][N:34]([CH3:36])[CH:35]=3)=[N:25]2)=[N:18][CH:19]=1.O>CC(C)=O>[OH:6][CH:3]([CH2:4][OH:5])[CH2:2][O:13][C:14]1[CH:15]=[N:16][C:17]([C:20]2[CH:21]=[C:22]([CH:37]=[CH:38][CH:39]=2)[CH2:23][N:24]2[C:29](=[O:30])[CH:28]=[CH:27][C:26]([C:31]3[CH:32]=[N:33][N:34]([CH3:36])[CH:35]=3)=[N:25]2)=[N:18][CH:19]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 72903-Chloro-1,2-propanediolHCID 10796Cesium carbonateHCID 59438049HCID 59438049, Verbindung

Produkt 1

HCID 46836756HCID 46836756, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

75 mg (0.68 mmol) of 3-chloro-1,2-propanediol and 322 mg (0.99 mmol) of caesium carbonate are added to 150 mg (0.41 mmol) of 2-[3-(5-hydroxy-pyrimidin-2-yl)benzyl]-6-(1-methyl-1H-pyrazol-4-yl)-2H-pyridazin-3-one, and the mixture is suspended in acetone. The reaction mixture is stirred at 80° C. for 5 days. Water is added to the reaction mixture, which is then extracted a number of times with ethyl acetate, dried over sodium sulfate and evaporated. The crude product is purified by means of column chromatography on silica gel.

Aufarbeitung

  1. extractionis then extracted a number of times with ethyl acetate
  2. dry with materialdried over sodium sulfate
  3. customevaporated
  4. customThe crude product is purified by means of column chromatography on silica gel

Quellen und Nachweise

ORD-Eintrag
ord-a35ed521ebe442eea318ef75896b3236
Quelldatensatz
uspto-grants-2014_01
Patentnummer
US08637518B2

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