反应详情

温度

170 °C

Add NaSEt (92 mg, 1.1 mmol) to a solution of 1-{2-[4-(10-methoxy-5H,7H-6-oxa-12-thia-dibenzo[a,e]azulen-7-yl)-phenoxy]-ethyl}-piperidine (266 mg, 0.55 mmol) in NMP (3 mL). Heat to 170° C. for 20 min. Add additional NaSEt (92 mg, 1.1 mmol) and continue heating for 1 h. Quench the reaction with water and dilute with CH2Cl2. Wash the organic phase with water and brine, dry over MgSO4, filter and concentrate. Purify the crude product by flash chromatography (0-10% (2M NH3 in MeOH)/CH2Cl2) followed by preparative HPLC to afford 7-[4-(2-piperidin-1-yl-ethoxy)-phenyl]-5H,7H-6-oxa-12-thia-dibenzo[a,e]azulen-10-ol (16.3 mg, 6.3%)

1. additionAdd additional NaSEt (92 mg, 1.1 mmol)
2. temperaturecontinue heating for 1 h
3. customQuench
4. customthe reaction with water
5. washWash the organic phase with water and brine
6. dry with materialdry over MgSO4
7. filtrationfilter
8. concentrationconcentrate
9. customPurify the crude product by flash chromatography (0-10% (2M NH3 in MeOH)/CH2Cl2)