反应详情

Sodium methanethiolate (0.23 g, 3.33 mmol) was dissolved in THF (1 ml) and added dropwise to a solution of 4-bromo-7-bromomethyl-2-isopropyl-2H-phthalazin-1-one (0.4 g, 1.11 mmol) in THF (10 ml). The mixture was stirred at RT for 3 hours whereupon LC-MS indicated complete consumption of starting material. The reaction mixture was diluted with water (20 ml) and extracted with EtOAc (50 ml). The organic layer was separated, dried (MgSO4), filtered and concentrated under vacuum. The residue was subjected to flash column chromatography (elution: 80% heptane, 20% EtOAc) to give the title compound (0.29 g, 79% yield) as a white solid.

1. customconsumption of starting material
2. additionThe reaction mixture was diluted with water (20 ml)
3. extractionextracted with EtOAc (50 ml)
4. customThe organic layer was separated
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated under vacuum
8. washThe residue was subjected to flash column chromatography (elution: 80% heptane, 20% EtOAc)