反应详情

To a 100 ml round-bottomed flask equipped with condenser and N2 inlet were added 1.22 g (3.52 mmol) (4-(4-(4-chlorobutyl)phenyl)-2-aminothiazole, 0.90 g (3.52 mmol) 3-piperazinyl-benzisothiazole, 1.84 ml (10.57 mmol) diisopropylethylamine, 0.75 g (7.04 mmol) sodium carbonate, 2 mg sodium iodide, and 35 ml methylisobutylketone. The reaction mixture was refluxed 6 days, cooled, and evaporated. The residue was chromatographed on silica gel using methylene chloride/ethyl acetate as eluent, and the product fractions dissolved in methylene chloride/methanol and precipitated by addition of methylene chloride saturated with HCl. The precipitate was filtered and dried to give a solid, 242 mg (13%), m.p. 258-261° C. NMR (DMSO-d6): 1.6-1.8 (m, 4H), 2.7 (t, 2H), 3.2-3.6 (m, 8H), 4.1 (m, 2H), 7.20 (s, 1H), 7.3-8.2 (m, 8H).

1. customTo a 100 ml round-bottomed flask equipped with condenser and N2 inlet
2. temperatureThe reaction mixture was refluxed 6 days
3. temperaturecooled
4. customevaporated
5. customThe residue was chromatographed on silica gel
6. dissolutionthe product fractions dissolved in methylene chloride/methanol
7. customprecipitated by addition of methylene chloride saturated with HCl
8. filtrationThe precipitate was filtered
9. customdried
10. customto give a solid, 242 mg (13%), m.p. 258-261° C