反应详情

(S)-7-(2-hydroxyethyl)-9-neopentyl-6,7,9,10-tetrahydroazepino[3,4-e]indazol-8(3H)-one (15 mg, 0.04 mmol) was dissolved in dichloromethane (1 mL). Thionyl chloride (100 μL) was added to the mixture. Reaction stirred at room temperature for 2 hours. Thionyl chloride (500 μL) was added to the mixture. Reaction stirred at room temperature for 2 hours and then was warmed to reflux for 2 hours. Reaction mixture was concentrated in vacuo. Residue was dissolved in acetonitrile (1 mL). Potassium carbonate (25 mg, 0.18 mmol) was added to the mixture followed by 3-(piperidin-4-yl)-3,4-dihydroquinazolin-2(1H)-one (16 mg, 0.07 mmol). Reaction was heated at reflux for 2 hours. Preparatory HPLC purification afforded the title compound as white solid in 25% yield. High resolution MS m/e (M+H)+=529.3282.

1. customReaction
2. customReaction
3. stirringstirred at room temperature for 2 hours
4. temperaturewas warmed
5. temperatureto reflux for 2 hours
6. customReaction mixture
7. concentrationwas concentrated in vacuo
8. dissolutionResidue was dissolved in acetonitrile (1 mL)
9. customReaction
10. temperaturewas heated
11. temperatureat reflux for 2 hours
12. customPreparatory HPLC purification