1-Hydroxy-2-naphthoic acid → HCID 178426857, Verbindung

HRID 384429

Reaktionsgleichung

Reaktionsgleichung von HRID 384429
[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.[OH:25][C:26]1[C:35]2[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH:29]=[CH:28][C:27]=1[C:36]([OH:38])=[O:37]>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.[OH:25][C:26]1[C:35]2[C:30](=[CH:31][CH:32]=[CH:33][CH:34]=2)[CH:29]=[CH:28][C:27]=1[C:36]([O-:38])=[O:37]

Komponenten

4

Edukt 2

HCID 68441-Hydroxy-2-naphthoic acidHCID 443879Tolterodine

Produkt 1

HCID 178426857HCID 178426857, VerbindungAusbeute 84,1 %

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 1.88 g of 1-hydroxy-2-naphthoic acid, which was suspended in 50 mL of acetone, and then stirred for 30 minutes. 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 4.32 g (theoretical yield: 84.1%) of the final product in light brown 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-59f8417dfb9c4d1388b21bd51a4d2e1e
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08367726B2

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