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 1H-Pyrrolo[2,3-b]pyridine (1, 0.455 g, 3.85 mmol) and 6-chloro-2-methoxypyridine-3-carbaldehyde (26, 0.661 g, 3.85 mmol) was added methanol (10 mL) followed by potassium hydroxide (0.310 g, 5.52 mmol). The reaction was allowed to stir at room temperature overnight. The reaction was extracted with diethyl ether/ethyl acetate and water. The organic layer was separated, dried over anhydrous magnesium sulfate, filtered and volatiles were removed by rotary evaporation to provide a solid that was treated with dichloromethane and stored in a freezer overnight. The white solid was collected by vacuum filtration and dried in vacuo to give 613 mg of compound 27 (2.12 mmol, 55%). MS(ESI) [M+H+]+=290.1.
WORKUP
后处理
- extractionThe reaction was extracted with diethyl ether/ethyl acetate and water
- customThe organic layer was separated
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customvolatiles were removed by rotary evaporation
- customto provide a solid
- waitstored in a freezer overnight
- filtrationThe white solid was collected by vacuum filtration
- customdried in vacuo