Reaktion #471608

Reaktionsgleichung

tolterodine

gentisic acid

→

final product

Ausbeute 42.5%

Tolterodine Gentisate

Ausbeute 42.5%

Lösungsmittel

acetone

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAcetone in the above mixture was removed by nitrogen
2. 2
   Temperaturreflux apparatus, and when about 10 20 mL of acetone
3. 3
   Sonstigewas removed there
4. 4
   workup.STIRRINGAfter stirring the mixture at room temperature (25° C.) for 1 hour
5. 5
   Filtrationthe solid precipitate was filtered
6. 6
   Waschenwashed with hexane
7. 7
   SonstigeThe resultant was dried at room temperature (25° C.) for 24 hours

Vorschrift

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.

Quelle