Sodium Carbonate → HCID 68644254, Verbindung

HRID 1158782Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1158782
C([O:8][C:9]1[CH:10]=[C:11]([CH:15]([OH:38])[CH2:16][N:17]([CH2:35][CH2:36]O)[C:18]([C:20]2[C:21]([C:29]3[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=3)=[N:22][C:23]([N:26]([CH3:28])[CH3:27])=[N:24][CH:25]=2)=[O:19])[CH:12]=[CH:13][CH:14]=1)C1C=CC=CC=1.C(=O)([O-])[O-].[Na+].[Na+]>>[CH3:27][N:26]([CH3:28])[C:23]1[N:22]=[C:21]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[C:20]([C:18]([N:17]2[CH2:35][CH2:36][O:38][CH:15]([C:11]3[CH:12]=[CH:13][CH:14]=[C:9]([OH:8])[CH:10]=3)[CH2:16]2)=[O:19])=[CH:25][N:24]=1

Komponenten

3

Edukt 2

HCID 10340Sodium CarbonateHCID 86610923HCID 86610923, Verbindung

Produkt 1

HCID 68644254HCID 68644254, VerbindungAusbeute 14,6 %

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To 2-dimethylamino-4-phenylpyrimidin-5-carboxylic acid [2-(3-benzyloxyphenyl)-2-hydroxyethyl]-(2-hydroxyethyl)amide (0.20 g, 0.39 mmol) 48% hydrogen bromide solution (4 ml) is added. The mixture is heated at 100° C. for 1 hour, cooled to room temperature, poured onto water and neutralized (pH 7) with sodium carbonate solution. The precipitate is filtered oft washed with water and dried. The crude product is chromatographed on silicagel using chloroform and chloroform-ethyl acetate 9:1 mixture as eluent. 0.023 g light-yellow title compound is obtained, m.p.: 140° C.

Aufarbeitung

  1. temperaturecooled to room temperature
  2. filtrationThe precipitate is filtered oft
  3. washwashed with water
  4. customdried
  5. customThe crude product is chromatographed on silicagel

Quellen und Nachweise

ORD-Eintrag
ord-d3badd827fa54996a8cd8fced8c8559d
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07812031B2

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