반응 #416586

반응 방정식

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

용매

methylisobutylketone

반응 조건

후처리

1. 1
   기타To a 125 ml round-bottomed flask equipped with condenser and N2 inlet
2. 2
   온도The reaction was heated
3. 3
   온도at reflux for 4.5 days
4. 4
   여과filtered hot
5. 5
   기타to remove inorganic material
6. 6
   온도cooled
7. 7
   여과the precipitate filtered
8. 8
   세척washed with ether and ethyl acetate
9. 9
   기타bubbled through
10. 10
    기타to precipitate the salt
11. 11
    여과the resulting solid filtered
12. 12
    세척washed with methylene chloride
13. 13
    기타dried
14. 14
    기타to give a solid, m.p. 170°-175° C., 1.93 g (51%)

실험 절차

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%).

출처