HRID2064523
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 4-dimethylamino-4-phenyl-1-[3-(2-triethylsilanyl-1H-pyrrolo[3,2-c]pyridin-3-yl)propyl]cyclohexanol (410 mg, 0.83 mmol) in anhydrous tetrahydrofuran (25 mL) was mixed with tetra-n-butyl ammonium fluoride trihydrate (1.05 g, 3.32 mmol) and boiled with reflux for 6 h. The reaction mixture was then concentrated to low volume in a vacuum and the raw product purified by means of flash chromatography (38 g, 20×2.5 cm) with ethyl acetate/methanol (2:1). The product was taken up in dichloromethane (40 mL), the solution dried with sodium sulphate and concentrated to low volume in a vacuum.
WORKUP
后处理
- temperaturewith reflux for 6 h
- concentrationThe reaction mixture was then concentrated to low volume in a vacuum
- customthe raw product purified by means of flash chromatography (38 g, 20×2.5 cm) with ethyl acetate/methanol (2:1)
- dry with materialthe solution dried with sodium sulphate
- concentrationconcentrated to low volume in a vacuum