Hydrochloric Acid → 6-Methoxy-8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromene-2-carboxylic acid hydrochloride

HRID 1795317Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1795317
C([O:3][C:4]([C:6]1[O:7][C:8]2[C:13]([C:14](=[O:16])[CH:15]=1)=[CH:12][C:11]([O:17][CH3:18])=[CH:10][C:9]=2[N:19]1[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]1)=[O:5])C.CO.[ClH:28]>>[ClH:28].[CH3:18][O:17][C:11]1[CH:12]=[C:13]2[C:8](=[C:9]([N:19]3[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]3)[CH:10]=1)[O:7][C:6]([C:4]([OH:5])=[O:3])=[CH:15][C:14]2=[O:16]

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 887MethanolHCID 22142223Ethyl-6-methoxy-8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromene-2-carboxylate

Produkt 1

HCID 692667556-Methoxy-8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromene-2-carboxylic acid hydrochloride

Versuchsvorschrift

Ethyl-6-methoxy-8-(4-Methyl-piperazin-1-yl)-4-oxo-4H-chromene-2-carboxylate (1.0 g. 2.89 mmol), as prepared in Reference Example 2d above, was suspended in 6 M HCl (60 ml) and methanol (10 mL) and warmed to reflux for 3.0 h. The reaction was allowed to cool. The solution was concentrated in vacuo and anhydrous toluene was added (×3) and the solution was again concentrated in vacuo. The residue was dried under vacuum (17 h) to yield 6-methoxy-8-(4-methyl-1-piperazinyl)-4-oxo-4H-chromene-2-carboxylic acid hydrochloride as a yellow powder (1.0 g, quantitative yield).

Aufarbeitung

  1. temperatureto reflux for 3.0 h
  2. temperatureto cool
  3. concentrationThe solution was concentrated in vacuo and anhydrous toluene
  4. additionwas added (×3)
  5. concentrationthe solution was again concentrated in vacuo
  6. customThe residue was dried under vacuum (17 h)

Quellen und Nachweise

ORD-Eintrag
ord-6677715055e440ef9843ba3645e10e4e
Quelldatensatz
uspto-grants-2006_04
Patentnummer
US07026314B2

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