HRID626715
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
A solution of [7-chloro-2-(2,6-dichlorophenyl)-2H-pyrazolo[4,3-c]pyridin-4-yl]-carbamic acid tert-butyl ester (531 mg, contaminated with residual tert-butyl carbamate) and TFA (10 mL) in DCM (10 mL) was stirred at room temperature for 2 h and then concentrated under reduced pressure. The residue was partitioned between ethyl acetate and sodium bicarbonate (sat. aq.). The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated to dryness under reduced pressure to afford the title compound as a beige solid (100 g, 30% yield over 2 steps). LCMS (Method D): RT=2.15 min, m/z: 313 [M+H+].
WORKUP
后处理
- concentrationconcentrated under reduced pressure
- customThe residue was partitioned between ethyl acetate and sodium bicarbonate (sat. aq.)
- washThe organic layer was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated to dryness under reduced pressure