反应详情

Combine 2-isopropyl-4,9-dihydro-3-thia-1,4,9-triaza-benzo[f]azulene-10-thione (2.61 g, 9.48 mmoles) with trifluoromethanesulfonic acid methyl ester (1.61 mL, 14.2 mmoles) in dichloromethane (20 mL). Stir at room temperature for 2 h, then remove solvent in vacuo. Suspend residue in pyridine (20 mL) and add (S)-2-(2-methoxyethyl)piperazine (1.37 g, 9.48 mmoles). Heat at 115° C. for 8 h, then remove solvent in vacuo and apply residue to silica gel column. Elute column with dichloromethane followed by 5% 2N ammonia-methanol in dichloromethane to obtain the title compound (2.11 g, 58%) as a yellow oil: mass spectrum (APCI): m/z=386.2 (M+1).

1. temperatureHeat at 115° C. for 8 h
2. washElute column with dichloromethane