反应详情

A solution of 1,3-benzothiazole-5-carbonitrile (100 mg, 0.62 mmol, 1.00 equiv) in sulfuric acid (3.0 mL) was heated for 2 h at 45° C. After cooling down, the reaction mixture was poured into 15 mL of water. The pH value of the solution was adjusted to 7 with saturated aqueous sodium bicarbonate. The resulting solution was extracted with of ethyl acetate (5×10.0 mL). The combined organic layers were washed with brine, dried over anhydrous sodium sulfate, filtered and then concentrated under vacuum. This resulted in 60.0 mg of the title compound as a crude product, which was used directly for next step without further purification. MS m/z [M+H]+ (ESI): 179.

1. temperatureAfter cooling down
2. extractionThe resulting solution was extracted with of ethyl acetate (5×10.0 mL)
3. washThe combined organic layers were washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated under vacuum