HRID588159
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
1-(6-chloro-3-methoxy-1-trityl-1H-pyrazolo[4,3-c]pyridin-4-yl)prop-2-yn-1-ol (257 mg, 0.535 mmol) was dissolved in DCM (5 ml) charged with Dess-MartinPeriodinane (341 mg, 0.803 mmol) and allowed to stir for 2 h at rt. The reaction was charged with 5 mL 1N sodium thiosulfate and 5 mL saturated sodium bicarbonate and allowed to stir for 15 minutes. The organic layer was separated and the solvents were concentrated in vacuo. Purification on silica gel, 10-50% EtOAc/hexanes gave 1-(6-chloro-3-methoxy-1-trityl-1H-pyrazolo[4,3-c]pyridin-4-yl)prop-2-yn-1-one (60B, 137 mg, 0.287 mmol, 53.5% yield). MS: [M+H]+ m/z 478.
WORKUP
后处理
- stirringto stir for 15 minutes
- customThe organic layer was separated
- concentrationthe solvents were concentrated in vacuo
- customPurification on silica gel, 10-50% EtOAc/hexanes