HRID131491

反应详情

EQUATION

反应方程式

HRID 131491 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customEvaporate the mixture uner reduced pressure
  2. temperaturereflux for 8 hours
  3. concentrationConcentrate the reaction mixture under reduced pressure
  4. additiondilute the residue with ethyl acetata
  5. washWash the organic with brine twice
  6. dry with materialdry over sodium sulfate
  7. filtrationfilter
  8. concentrationconcentrate under reduced pressure
  9. customto give a residue
  10. customPurify the residue by flash chromatography
  11. washeluting with 2M ammonia in methanol:dichloromethane (5:95)