تفاعل #218673

معادلة التفاعل

pyridine

2-isopropyl-4,9-dihydro-3-thia-1,4,9-triaza-benzo[f]azulene-10-thione

methyl triflate

(S)-2-(3-methoxy-propyl)-piperazine

→

title compound

(S)-10-[3-(3-Methoxy-propyl)-piperazin-1-yl]-2-isopropyl-4H-3-thia-1,4,9-triaza-benzo[f]azulene

المذيبات

dichloromethane

ظروف التفاعل

المعالجة

1. 1
   أخرىEvaporate the mixture uner reduced pressure
2. 2
   درجة الحرارةreflux for 8 hours
3. 3
   تركيزConcentrate the reaction mixture under reduced pressure
4. 4
   workup.ADDITIONdilute the residue with ethyl acetata
5. 5
   غسيلWash the organic with brine twice
6. 6
   تجفيفdry over sodium sulfate
7. 7
   ترشيحfilter
8. 8
   تركيزconcentrate under reduced pressure
9. 9
   أخرىto give a residue
10. 10
    أخرىPurify the residue by flash chromatography
11. 11
    غسيلeluting with 2M ammonia in methanol:dichloromethane (5:95)

الإجراء التجريبي

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).

المصدر