Reaktion #716776

Reaktionsgleichung

4-chloro-3-nitrobenzenesulfonamide

mixture

1-(tetrahydro-2H-pyran-4-yl)piperidin-4-amine

water

triethylamine

→

3-nitro-4-(1-(tetrahydro-2H-pyran-4-yl)piperidin-4-ylamino)benzenesulfonamide

Lösungsmittel

1,4-dioxane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISSOLUTIONcompletely dissolved
2. 2
   Temperaturcooled
3. 3
   Einengenconcentrated
4. 4
   workup.ADDITION10% methanol in dichloromethane was added
5. 5
   Filtrationthe mixture was filtered

Vorschrift

A mixture of EXAMPLE 173B (22.12 g), water (43 mL), and triethylamine (43.6 mL) in 1,4-dioxane (300 mL) was stirred at room temperature until EXAMPLE 173B completely dissolved. The solution was then treated with 4-chloro-3-nitrobenzenesulfonamide, heated at 90° C. for 16 hours, cooled and concentrated. 10% methanol in dichloromethane was added, and the solution was stirred vigorously at room temperature until a fine suspension existed and the mixture was filtered.

Quelle