反应详情

温度

90 °C

Suspend 6-fluoro-2-methyl-4,9-dihydro-3-thia-4,9-diazabenzo[f]azulene-10-thione (500 mg, 1.9 mmol) in dichloromethane (30 ml), stir under nitrogen and cool in an ice/water bath. Add methyl trifluoromethanesulfonate (500 μl), and stir overnight. Concentrate the reaction mixture under reduced pressure, take up in pyridine (10 ml) and add (S)-2-(2-methoxyethyl)piperazine (400 mg, 2.78 mmol) and stir the reaction mixture under nitrogen and heat at 90° C. for three days. Concentrate the reaction mixture under reduced pressure and purify by flash column chromatography on silica gel (eluent dichloromethane/methanol) to give the desired as a yellow solid 727 mg: Mass Spectrum (FIA) 375 (M+1).

1. temperaturecool in an ice/water bath
2. concentrationConcentrate the reaction mixture under reduced pressure
3. stirringstir the reaction mixture under nitrogen
4. concentrationConcentrate the reaction mixture under reduced pressure
5. custompurify by flash column chromatography on silica gel (eluent dichloromethane/methanol)
6. customto give the