反应详情

0.2 g 2-(2,4-Dichloro-6-fluorobenzothiazol-7-yl)1,3,4,5,6,7-hexahydro-2H-indazol-3-one was treated with 2 ml phosphorus oxychloride and the mixture stirred for one hour under reflux. After cooling, it was poured into ice-water, extracted with ethyl acetate and the organic phase washed with sodium hydrogen carbonate and water. It was dried over magnesium sulfate and concentrated. The residue was purified by column chromatography. Yield: 0.07 g=32% of theory m.p.: 161°-163° C.

1. temperatureunder reflux
2. temperatureAfter cooling
3. extractionextracted with ethyl acetate
4. washthe organic phase washed with sodium hydrogen carbonate and water
5. dry with materialIt was dried over magnesium sulfate
6. concentrationconcentrated
7. customThe residue was purified by column chromatography