反应详情

A mixture of 5-chloro-3-p-tolyl-1,2,4-thiadiazole (900 mg, 4.27 mmol) and piperazine (1.84 g, 21.4 mmol) in 25 mL EtOH were heated to reflux and stirred for 1 h at this temperature. The resulting yellow solution was cooled to room temperature and concentrated in vacuo. The residue was purified by flash column chromatography on silica eluting with a gradient formed from DCM, MeOH and NEt3 to yield after evaporation of the product containing fractions 1.1 g (99%) of the title compound as light yellow solid. MS (m/e): 261.3 (MH+).

1. temperaturewere heated
2. temperatureto reflux
3. concentrationconcentrated in vacuo
4. customThe residue was purified by flash column chromatography on silica eluting with a gradient
5. customformed from DCM, MeOH and NEt3
6. customto yield
7. customafter evaporation of the product
8. additioncontaining fractions 1.1 g (99%) of the title compound as light yellow solid