反应详情

Combine 2-methyl-4,9-dihydro-3-thia-4,9-diazabenzo[f]azulene-10-thione (0.382 g 1.55 mmol), (S)-2-(2-phenoxyethyl)piperazine (0.320 g, 1.55 mmol) and pyridine (5 mL) and reflux for 36 hours. Evaporate the mixture and apply the material to 10 g of SCX, then elute with methanol followed by 5% 2N ammonia-methanol in dichloromethane and then 2N ammonia-methanol. Purification by flash chromatography, eluting with a step gradient starting with dichloromethane going to 7% 2N ammonia-methanol in dichloromethane gives the title compound: mass spectrum (APCI): m/z=419.1 (M+1).

1. customEvaporate the mixture
2. washapply the material to 10 g of SCX, then elute with methanol
3. customPurification by flash chromatography
4. washeluting with a step gradient