反应详情

温度

60 °C

10 g of 2-chloro-6-trifluoromethoxybenzothiazole are added dropwise over one hour to a mixture, cooled to 10° C., of concentrated sulphuric acid (50 cm3) and concentrated nitric acid (25 cm3). The mixture is then heated for one hour at 60° C. After cooling, the mixture is poured into an ice/water mixture (1/1 by weight) and extracted with 3 times 100 cm3 of chloroform. The organic phases are dried over magnesium sulphate and concentrated under vacuum (2.7 kPa). The residue is purified by flash chromatography with a chloroform/cyclohexane mixture (4/6 by volume) as eluent. 6.4 g of 2-chloro-7-nitro-6-trifluoromethoxybenzothiazole are thus obtained, melting at 64° C.

1. temperatureAfter cooling
2. extractionextracted with 3 times 100 cm3 of chloroform
3. dry with materialThe organic phases are dried over magnesium sulphate
4. concentrationconcentrated under vacuum (2.7 kPa)
5. customThe residue is purified by flash chromatography with a chloroform/cyclohexane mixture (4/6 by volume) as eluent