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2,5-Dihydroxybenzoic acid → HCID 178426858, Verbindung

HRID 384426
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 384426
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([OH:24])=[C:6]([C@@H:8]([C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH2:9][CH2:10][N:11]([CH:15]([CH3:17])[CH3:16])[CH:12]([CH3:14])[CH3:13])[CH:7]=1.[C:25]([OH:35])(=[O:34])[C:26]1[C:27](=[CH:29][CH:30]=[C:31]([CH:33]=1)[OH:32])[OH:28]>CC(C)=O>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([OH:24])=[C:6]([C@@H:8]([C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=2)[CH2:9][CH2:10][N:11]([CH:12]([CH3:14])[CH3:13])[CH:15]([CH3:16])[CH3:17])[CH:7]=1.[C:25]([O-:35])(=[O:34])[C:26]1[C:27](=[CH:29][CH:30]=[C:31]([CH:33]=1)[OH:32])[OH:28]
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Komponenten

4

Edukt 2

HCID 34692,5-Dihydroxybenzoic acidHCID 443879Tolterodine

Produkt 1

HCID 178426858HCID 178426858, VerbindungAusbeute 42,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 180AcetoneLösungsmittel2×

Versuchsvorschrift

3.25 g of tolterodine dissolved in 50 mL of acetone was mixed at room temperature (25° C.) with 4.80 g of gentisic acid, which was suspended in 50 mL of acetone, and then stirred. Acetone in the above mixture was removed by nitrogen reflux apparatus, and when about 10 20 mL of acetone was removed there started to appear a solid precipitate. After stirring the mixture at room temperature (25° C.) for 1 hour, the solid precipitate was filtered and then washed with hexane. The resultant was dried at room temperature (25° C.) for 24 hours and 2.04 g (theoretical yield: 42.5%) of the final product in white solid was obtained.

Aufarbeitung

  1. customAcetone in the above mixture was removed by nitrogen
  2. temperaturereflux apparatus, and when about 10 20 mL of acetone
  3. customwas removed there
  4. stirringAfter stirring the mixture at room temperature (25° C.) for 1 hour
  5. filtrationthe solid precipitate was filtered
  6. washwashed with hexane
  7. customThe resultant was dried at room temperature (25° C.) for 24 hours

Quellen und Nachweise

ORD-Eintrag
ord-e381d6cfd33c4dde97db0152e45ecbce
Quelldatensatz
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08367726B2

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