反应详情

温度

160 °C

To a solution of 6-bromo-2-(4-cyclopentylpiperazin-1-yl)benzothiazole (0.54 g, 1.50 mmol) in N-methylpyrrolidin-2-one (100 mL) was added copper(I)iodide (344 mg, 1.80 mmol) and copper(I)cyanide (270 mg, 3.0 mmol). The mixture was heated at 160° C. for 4 h, then allowed to cool to room temperature and filtered. The filtercake was washed with ethyl acetate and the filtrate was extracted with ethyl acetate. The combined organic extracts were washed with brine, dried (Na2SO4) and concentrated under reduced pressure. The residue was purified by preparative HPLC to afford 140 mg (30%) of 2-(4-cyclopentylpiperazin-1-yl)benzothiazole-6-carbonitrile.

1. temperatureto cool to room temperature
2. filtrationfiltered
3. washThe filtercake was washed with ethyl acetate
4. extractionthe filtrate was extracted with ethyl acetate
5. washThe combined organic extracts were washed with brine
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated under reduced pressure
8. customThe residue was purified by preparative HPLC