HRID634391
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
The title compound was made in a similar way as that of the intermediate C6, using 3-(1-hydroxyethyl)-4-(6-methylpyridin-3-yl)-1H-isochromen-1-one intermediate B10 (163 mg, 0.579 mmol), 1M PBr3 (0.87 mL, 0.87 mmol) in a mixture of DCM (2 ml) and DMF (3 ml) at RT. The crude was purified via reverse phase chromatography with a Biotage C18 SNAP 60 g column (Phase A, water 95%, ACN 4.9%, formic acid 0.1%); Phase B ACN 99.9%, formic acid 0.1%). The aqueous fractions were added of 50% HBraqueous and concentrated under reduced pressure to give the title compound (320 mg).
WORKUP
后处理
- customThe crude was purified via reverse phase chromatography with a Biotage C18 SNAP 60 g column (Phase A, water 95%, ACN 4.9%, formic acid 0.1%)
- additionThe aqueous fractions were added of 50% HBraqueous
- concentrationconcentrated under reduced pressure