HRID861143
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
To a solution of 1-[7-chloro-2-(3-methylphenyl)pyrazolo[1,5-a]pyridin-3-yl]-2-propyn-1-ol (11.3 g, 36.2 mmol) in chloroform (300 mL) was added manganese dioxide (78.9 g, 905 mmol). The reaction mixture was stirred at room temperature for 18 hours. The suspension was filtered through a pad of Celite and the filtrate was concentrated and purified by flash chromatography (7:3 hexanes:ethyl acetate). 1-[7-chloro-2-(3-methylphenyl)pyrazolo[1,5-a]pyridin-3-yl]-2-propyn-1-one (4.57 g, 41%) was obtained as a pale yellow crystalline. 1H NMR (CDCl3) δ 8.48 (d, 1H), 7.51 (m, 3H), 7.33 (t, 1H), 7.29 (d, 1H), 8.21 (dd, 1H), 2.89 (s, 1H), 2.42 (s, 3H); MS m/z 295 (M+1).
WORKUP
后处理
- filtrationThe suspension was filtered through a pad of Celite
- concentrationthe filtrate was concentrated
- custompurified by flash chromatography (7:3 hexanes:ethyl acetate)