Reaktion #62941

Reaktionsgleichung

6-bromo-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-5-one, hydrobromide

thiourea

→

title compound

Ausbeute 92.8%

5,6-Dihydro-4H-thiazolo[4',5':3,4]cyclohepta[1,2-b]pyridin-2-amine

Ausbeute 92.8%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   FiltrationThe mixture is filtered hot through a pad of Celite
2. 2
   Sonstigeto remove a small amount of insoluble solid
3. 3
   TemperaturThe filtrate is cooled
4. 4
   Sonstigea precipitate is collected
5. 5
   SonstigeRecrystallization from acetonitrile

Vorschrift

A solution of 6.78 g (21.12 mmol) of 6-bromo-6,7,8,9-tetrahydro-5H-cyclohepta[b]pyridin-5-one, hydrobromide and 1.93 g (25.35 mmol) of thiourea in 100 ml of water is heated on a steam bath for 2 hours. The mixture is filtered hot through a pad of Celite to remove a small amount of insoluble solid. The filtrate is cooled, basified with ammonium hydroxide, and a precipitate is collected. Recrystallization from acetonitrile affords 4.26 g (92.8%) of the title compound as a tan solid; mp 220°-222° C. (dec.).

Quelle