반응 #218627

반응 방정식

6-fluoro-2-methyl-4,9-dihydro-3-thia-4,9-diazabenzo[f]azulene-10-thione

methyl trifluoromethanesulfonate

(S)-2-(2-methoxyethyl)piperazine

→

(S)-6-Fluoro-10-[3-(2-methoxy-ethyl)-piperazin-1-yl]-2-methyl-4H-3-thia-4,9-diaza-benzo[f]azulene

용매

dichloromethane

반응 조건

후처리

1. 1
   온도cool in an ice/water bath
2. 2
   농축Concentrate the reaction mixture under reduced pressure
3. 3
   workup.STIRRINGstir the reaction mixture under nitrogen
4. 4
   농축Concentrate the reaction mixture under reduced pressure
5. 5
   기타purify by flash column chromatography on silica gel (eluent dichloromethane/methanol)
6. 6
   기타to give the

실험 절차

Suspend 6-fluoro-2-methyl-4,9-dihydro-3-thia-4,9-diazabenzo[f]azulene-10-thione (500 mg, 1.9 mmol) in dichloromethane (30 ml), stir under nitrogen and cool in an ice/water bath. Add methyl trifluoromethanesulfonate (500 μl), and stir overnight. Concentrate the reaction mixture under reduced pressure, take up in pyridine (10 ml) and add (S)-2-(2-methoxyethyl)piperazine (400 mg, 2.78 mmol) and stir the reaction mixture under nitrogen and heat at 90° C. for three days. Concentrate the reaction mixture under reduced pressure and purify by flash column chromatography on silica gel (eluent dichloromethane/methanol) to give the desired as a yellow solid 727 mg: Mass Spectrum (FIA) 375 (M+1).

출처