反应详情

温度

45 °C

2.0 g (6.55 mmol) 3-(4-bromo-phenyl)-benzo[d]isothiazol-6-ol in 30 ml acetone were treated with 5.89 g (42.5 mmol, 6.5 eq) K2CO3 and 1.9 ml (16.33 mmol, 2.5 eq) 1,4-dibromobutane. The reaction mixture was stirred at 45° C. for 8 h and at RT over night, filtered and evaporated. The excess of dibromide was removed in vacuo and the crude product was purified by column chromatography on silica gel with a gradient EtOAc:hexane 1:9 to 1:4 to yield 2.0 g (71%) 6-(4-Bromo-butoxy)-3-(4-bromo-phenyl)-benzo[d]isothiazole as yellow semisolid, MS: 439 (M, 2Br).

1. filtrationfiltered
2. customevaporated
3. customThe excess of dibromide was removed in vacuo
4. customthe crude product was purified by column chromatography on silica gel with a gradient EtOAc:hexane 1:9 to 1:4