HRID1890635
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
{4-[3-(2-Ethyl-5,7-dimethylimidazo[4,5-b]pyridin-3-ylmethyl)benzoyl]benzyloxy)-tert-butyldimethylsilane (0.898 g, 1.75 mmol) obtained in Step 4 was dissolved in THF (15 mL), and a 1.0 mol/L TBAF-THF solution (5.24 mL, 5.24 mmol) was added to the solution, followed by stirring at room temperature for 2 hours. The reaction mixture was diluted with ethyl acetate, and washed with water and saturated brine. The organic layer was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate:hexane=2:1), followed by crystallization from ethanol to obtain Compound 14 (0.579 g, yield 83%).
WORKUP
后处理
- washwashed with water and saturated brine
- dry with materialThe organic layer was dried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure
- customThe residue was purified by silica gel column chromatography (ethyl acetate:hexane=2:1)
- customfollowed by crystallization from ethanol