Reaktion #446623

Reaktionsgleichung

1-(6-chloro-3-pyridazinyl)-4-(3-methoxyphenyl)-4-piperidinol

hydrochloric acid

→

3-chloro-6-[3,6-dihydro-4-(3-methoxyphenyl)-1(2H)-pyridinyl]pyridazine

Ausbeute 64.0%

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturat reflux temperature
2. 2
   SonstigeThe reaction mixture was evaporated
3. 3
   workup.ADDITIONWater was added
4. 4
   workup.ADDITIONthe whole was treated with concentrate ammonium hydroxide
5. 5
   ExtraktionThe product was extracted with trichloromethane
6. 6
   SonstigeThe extract was dried
7. 7
   Filtrationfiltered
8. 8
   Sonstigeevaporated
9. 9
   SonstigeThe residue was crystallized from 2-propanol
10. 10
    FiltrationThe product was filtered off
11. 11
    Sonstigedried

Vorschrift

A mixture of 4 parts of 1-(6-chloro-3-pyridazinyl)-4-(3-methoxyphenyl)-4-piperidinol, 80 parts of ethanol and 50 parts of a hydrochloric acid solution 6 N was stirred for 6 hours at reflux temperature. The reaction mixture was evaporated. Water was added and the whole was treated with concentrate ammonium hydroxide. The product was extracted with trichloromethane. The extract was dried, filtered and evaporated. The residue was crystallized from 2-propanol. The product was filtered off and dried, yielding 2.5 parts (64%) of 3-chloro-6-[3,6-dihydro-4-(3-methoxyphenyl)-1(2H)-pyridinyl]pyridazine; mp. 126.4° C. (compound 235).

Quelle