Reaktion #2000681

Reaktionsgleichung

compound

2-Amino-6-({[2-(4-chlorophenyl)-1,3-thiazol-4-yl]methyl}thio)-4-(methylthio)pyridine-3,5-dicarbonitrile

piperidine

ammonium chloride

ethyl acetate

→

2-Amino-6-({[2-(4-chlorophenyl)-1,3-thiazol-4-yl]methyl}sulfanyl)-4-piperidin-1-ylpyridine-3,5-dicarbonitrile

Lösungsmittel

acetone

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   Temperaturat reflux for 8 h
3. 3
   TemperaturAfter cooling
4. 4
   SonstigeThe phases were separated
5. 5
   WaschenThe organic phase was washed twice with in each case 20 ml of saturated aqueous sodium chloride solution
6. 6
   Trocknendried over magnesium sulfate
7. 7
   SonstigeAfter removal of the solvent
8. 8
   Sonstigethe residue was triturated with 100 ml of diethyl ether
9. 9
   FiltrationThe precipitate was filtered off with suction
10. 10
    Sonstigedried under reduced pressure at 50° C.

Vorschrift

5.00 g (11.63 mmol) of the compound from Example 44A and 57.50 ml (581.43 mmol) of piperidine were initially charged in 120 ml of acetone and heated at reflux for 8 h. After cooling, the mixture was poured into a solvent mixture of 50 ml of saturated aqueous ammonium chloride solution and 50 ml of ethyl acetate. The phases were separated. The organic phase was washed twice with in each case 20 ml of saturated aqueous sodium chloride solution and then dried over magnesium sulfate. After removal of the solvent, the residue was triturated with 100 ml of diethyl ether. The precipitate was filtered off with suction and dried under reduced pressure at 50° C.

Quelle