Hydrochloric Acid → HCID 22640027, Verbindung

HRID 2415103

Reaktionsgleichung

Reaktionsgleichung von HRID 2415103
C([O:8][C:9]1[CH:10]=[C:11]([CH:23]=[CH:24][C:25]=1[O:26][CH3:27])[CH2:12][NH:13][C:14]1[C:19]([Cl:20])=[C:18]([CH3:21])[N:17]=[C:16]([CH3:22])[N:15]=1)C1C=CC=CC=1.Cl>C(O)C>[Cl:20][C:19]1[C:14]([NH:13][CH2:12][C:11]2[CH:23]=[CH:24][C:25]([O:26][CH3:27])=[C:9]([OH:8])[CH:10]=2)=[N:15][C:16]([CH3:22])=[N:17][C:18]=1[CH3:21]

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 22639999(3-Benzyloxy-4-methoxybenzyl)(5-chloro-2,6-dimethylpyrimidin-4-yl)amine

Produkt 1

HCID 22640027HCID 22640027, VerbindungAusbeute 81,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

In analogy to the method described in example B1, 3.0 g (7.8 mmol) of (3-benzyloxy-4-methoxy-benzyl)(5-chloro-2,6-dimethylpyrimidin-4-yl)amine (from example A4) are reacted with 30 ml of 12.5N hydrochloric acid in 30 ml of ethanol. Extraction with ethyl acetate at a pH of 8 gives, after concentration, a solid residue which is chromatographed on silica gel (mobile phase: toluene/dioxane=5:1). Crystallization from toluene/methanol gives 1.86 g (72%) of the title compound as a beige crystallizate. m.p.: 165-168° C.

Aufarbeitung

  1. extractionExtraction with ethyl acetate at a pH of 8
  2. customgives
  3. concentrationafter concentration
  4. customa solid residue which is chromatographed on silica gel (mobile phase: toluene/dioxane=5:1)
  5. customCrystallization from toluene/methanol

Quellen und Nachweise

ORD-Eintrag
ord-06d98458d60647c4a9c22b5e250ddeec
Quelldatensatz
uspto-grants-2004_11
Patentnummer
US06818642B2

Verknüpfte Notizen

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