反应详情

温度

0 °C

Sodium hydride (1.05 equiv.) was added to a 0° C. DMF solution (0.14 M) of propyl {(7R)-7-{[(4-fluorophenyl)sulfonyl]amino}-6,7,8,9-tetrahydropyrido [1,2-α]indol-10-yl }acetate from Step 7 and the mixture was stirred at 0 ° C. for 30 min. lodomethane (3 equiv.) was added and the reaction was stirred at 0° C. for 2 h. The mixture was poured in aqueous NH4Cl and extracted with Et2O (2×). The combined organic extracts were washed with water (3×), brine and then dried with MgSO4, filtered and concentrated under vacuum. The residue was purified by column chromatography on silica gel using a CombiFlashRF (Teledyne ISCO) eluting with EtOAc/Hex (5:95 to 50:50) to give the title compound (98%) as a colorless oil.

1. additionwas added
2. extractionextracted with Et2O (2×)
3. washThe combined organic extracts were washed with water (3×), brine
4. dry with materialdried with MgSO4
5. filtrationfiltered
6. concentrationconcentrated under vacuum
7. customThe residue was purified by column chromatography on silica gel using a CombiFlashRF (Teledyne ISCO)
8. washeluting with EtOAc/Hex (5:95 to 50:50)