反应详情

Combine 3-[4-(3-bromo-propoxy)-phenyl]-benzo[b]thiophene (0.200 g, 0.576 mmol), 2-chlorobenzylamine (0.326 g, 2.30 mmol), potassium carbonate (0.200 g, 1.45 mmol) and acetonitrile (4.0 ml) and heat (75° C.) overnight. Cool reaction to room temperature, filter through a Waters Sep-Pak 1 g Silica cartridge (ethyl acetate) and concentrate (in vacuo). Purify the crude product by column (silica) chromatography with a graded solvent mixture of 40% ethyl acetate in dichloromethane to 100% ethyl acetate. Concentrate the appropriate fractions, dissolve in dichloromethane and re-evaporate under a stream of nitrogen. Dry sample under vacuum (0.5 mm Hg, 50° C.) overnight to obtain the title compound as a light amber oil (0.184 g, 78% Yield). Purity by LC/MS=98%, [M+H]+=408.

1. temperatureCool
2. customreaction to room temperature
3. filtrationfilter through a Waters Sep-Pak 1 g Silica cartridge (ethyl acetate)
4. concentrationconcentrate (in vacuo)
5. customPurify the crude product by column (silica) chromatography
6. additionwith a graded solvent mixture of 40% ethyl acetate in dichloromethane to 100% ethyl acetate
7. concentrationConcentrate the appropriate fractions
8. dissolutiondissolve in dichloromethane
9. customre-evaporate under a stream of nitrogen
10. customDry sample under vacuum (0.5 mm Hg, 50° C.) overnight