반응 #416584

반응 방정식

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

N-(1-naphthyl)piperazine

diisopropylethylamine

sodium carbonate

sodium iodide

→

4-(4-(2-(4-(1-Naphthyl)piperazinyl)ethyl)phenyl)-2-methylaminothiazole

용매

methylene chloride

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 days
4. 4
   온도cooled
5. 5
   여과the precipitate filtered
6. 6
   기타the filtrate evaporated
7. 7
   기타chromatographed on silica gel
8. 8
   기타to give an oil
9. 9
   기타precipitated by addition of methylene chloride saturated with hydrochloride
10. 10
    여과the precipitate filtered
11. 11
    세척washed with ether
12. 12
    기타dried
13. 13
    기타to give a white solid, m.p. 272°-273° C., 2.37 g (63%)

실험 절차

To a 125 ml round-bottomed flask equipped with condenser and N2 inlet were added 2.50 g (7.5 mmol) of 4-(4-(2-chloroethyl)phenyl)-2-methylaminothiazole hydrobromide, 1.59 g (7.5 mmol) of N-(1-naphthyl)piperazine, 1.31 ml (7.5 mmol) of diisopropylethylamine, 1.59 g (15 mmol) of sodium carbonate, 5 mg of sodium iodide, and 50 ml of methylisobutylketone. The reaction was heated at reflux for 4 days, cooled, and the precipitate filtered, and the filtrate evaporated. The residue was taken up in methylene chloride and chromatographed on silica gel using methylene chloride/ethyl acetate as eluent to give an oil. The oil was taken up in methylene chloride, precipitated by addition of methylene chloride saturated with hydrochloride, and the precipitate filtered, washed with ether, and dried to give a white solid, m.p. 272°-273° C., 2.37 g (63%).

출처