Reaktion #75150

Reaktionsgleichung

4-chloro-1,3-dihydro-3-(3-hydroxypropyl)-2H-benzimidazol-2-one methane sulfonate

1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one

sodium carbonate

4-methyl-2-pentanone

→

8-[3-(7-chloro-1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one

Ausbeute 17.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturrefluxed overnight
2. 2
   TemperaturThe reaction mixture is cooled
3. 3
   FiltrationThe precipitated product is filtered off
4. 4
   Sonstigecrystallized twice from a mixture of N,N-dimethylformamide and water

Vorschrift

A mixture of 4.2 parts of 4-chloro-1,3-dihydro-3-(3-hydroxypropyl)-2H-benzimidazol-2-one methane sulfonate, 2.5 parts of 1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one, 10 parts of sodium carbonate and 80 parts of 4-methyl-2-pentanone is stirred and refluxed overnight. The reaction mixture is cooled and water is added. The precipitated product is filtered off and crystallized twice from a mixture of N,N-dimethylformamide and water, yielding 0.8 parts (17%) of 8-[3-(7-chloro-1,3-dihydro-2-oxo-2H-benzimidazol-1-yl)propyl]-1-phenyl-1,3,8-triazaspiro[4,5]decan-4-one; mp. 258.4° C.

Quelle