Reaktion #416586

Reaktionsgleichung

4-(4-(2-chloroethyl)phenyl)-2-methylthiazole hydrobromide

N-(3-trifluoromethylphenyl)piperazine hydrochloride

diisopropylethylamine

sodium carbonate

sodium iodide

→

4-(4-(2-(4-(3-Trifluoromethylphenyl)piperazinyl)ethyl)phenyl)-2-methylthiazole

Lösungsmittel

methylisobutylketone

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 125 ml round-bottomed flask equipped with condenser and N2 inlet
2. 2
   TemperaturThe reaction was heated
3. 3
   Temperaturat reflux for 4.5 days
4. 4
   Filtrationfiltered hot
5. 5
   Sonstigeto remove inorganic material
6. 6
   Temperaturcooled
7. 7
   Filtrationthe precipitate filtered
8. 8
   Waschenwashed with ether and ethyl acetate
9. 9
   Sonstigebubbled through
10. 10
    Sonstigeto precipitate the salt
11. 11
    Filtrationthe resulting solid filtered
12. 12
    Waschenwashed with methylene chloride
13. 13
    Sonstigedried
14. 14
    Sonstigeto give a solid, m.p. 170°-175° C., 1.93 g (51%)

Vorschrift

To a 125 ml round-bottomed flask equipped with condenser and N2 inlet were added 2.39 g (7.5 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-methylthiazole hydrobromide, 2.0 g (7.5 mmol) of N-(3-trifluoromethylphenyl)piperazine hydrochloride, 2.62 ml (15.0 mmol) of diisopropylethylamine, 1.59 g (15.0 mmol) of sodium carbonate, 5 mg of sodium iodide, and 50 ml of methylisobutylketone. The reaction was heated at reflux for 4.5 days, filtered hot to remove inorganic material, cooled, and the precipitate filtered and washed with ether and ethyl acetate. The solid was taken up in methylene chloride, hydrochloride gas bubbled through to precipitate the salt, and the resulting solid filtered, washed with methylene chloride, and dried to give a solid, m.p. 170°-175° C., 1.93 g (51%).

Quelle