反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Combine 2-isopropyl-4,9-dihydro-3-thia-1,4,9-triaza-benzo[f]azulene-10-thione (0.5 g, 1.816 mmol), methyl triflate (0.306 mL, 2.723 mmol) in dichloromethane (4 mL) and stir at ambient temperature for 2 hours. Evaporate the mixture uner reduced pressure and then combine the residue with (S)-2-(3-methoxy-propyl)-piperazine (0.287 g, 1.816 mmol) and pyridine (4 mL) and reflux for 8 hours. Concentrate the reaction mixture under reduced pressure and dilute the residue with ethyl acetata. Wash the organic with brine twice, dry over sodium sulfate, filter and concentrate under reduced pressure to give a residue. Purify the residue by flash chromatography, eluting with 2M ammonia in methanol:dichloromethane (5:95) to give the title compound: mass spectrum (m/e):400.03 (M+1).
WORKUP
后处理
- customEvaporate the mixture uner reduced pressure
- temperaturereflux for 8 hours
- concentrationConcentrate the reaction mixture under reduced pressure
- additiondilute the residue with ethyl acetata
- washWash the organic with brine twice
- dry with materialdry over sodium sulfate
- filtrationfilter
- concentrationconcentrate under reduced pressure
- customto give a residue
- customPurify the residue by flash chromatography
- washeluting with 2M ammonia in methanol:dichloromethane (5:95)