反应详情

Stir 2-isopropyl-4,9-dihydro-3-thia-1,4,9-triaza-benzo[f]azulene-10-thione (0.551 g, 2.0 mmol) in dichloromethane (10.0 mL) and chilled in an ice bath while adding methyl trifluoromethane sulfonate (0.27 mL, 2.4 mmol). Allow this solution to stir at ambient temperature for 16 hours. Evaporate the solvent to a gray solid. Dissolve this solid and (S)-2-[2-(4-fluoro-phenyl)-ethyl]-piperazine (0.417 g, 2.0 mmol) in pyridine (8.0 mL) and heat at 115° C. for 23 hours. After evaporation of the pyridine, silica gel chromatography, eluting with methylene chloride: 2N NH3/methanol (100:5), gives 0.354 g of the title compound as a yellow solid: mass spectrum (ion spray): m/z=450 (M+1); Analysis for C25H28FN5S(0.2 H2O): calcd: C, 66.26; H, 6.32; N, 15.45; found: C, 66.01; H, 6.15; N, 15.25.

1. temperaturechilled in an ice bath
2. customEvaporate the solvent to a gray solid
3. temperatureheat at 115° C. for 23 hours
4. customAfter evaporation of the pyridine, silica gel chromatography
5. washeluting with methylene chloride