反应详情

温度

0 °C

6-fluorobenzo[d]thiazole-2-thiol (14.0 g, 0.075 mol) was suspended in dry DCM (100 mL) under nitrogen and cooled to 0° C. Sulfuryl chloride (18.5 mL) was then added dropwise and the reaction was allowed to warm to RT and stirred for 1 h. The reaction mixture was then poured on to crushed ice and extracted with DCM (4×300 mL). The combined organic extract was given brine wash (2×150 mL), dried (Na2SO4) and concentrated. The crude compound was purified by column chromatography (Silica 100-200 mesh; 3-7% ethyl acetate in hexane) to provide 2-chloro-6-fluorobenzo[d]thiazole as a white solid.

1. temperatureto warm to RT
2. additionThe reaction mixture was then poured on
3. customto crushed ice
4. extractionextracted with DCM (4×300 mL)
5. extractionThe combined organic extract
6. washwash (2×150 mL)
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated
9. customThe crude compound was purified by column chromatography (Silica 100-200 mesh; 3-7% ethyl acetate in hexane)