HRID2356387
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
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
A mixture of 2-ethyl-6-fluoro-3-piperidin-4-yl-1H-indole (0.9 g), 1-(3-Bromo-propylsulfanyl)-4-fluoro-benzene (1.0 g), potassium iodide (20 mg) and potassium carbonate (0.7 g) in DMF (10 ml) is heated at 100° C. for 3 h, and allowed to cool to rt overnight. Ethyl acetate (50 ml) and water (25 ml) are added and the organic phase is washed with water, dried and concentrated in vacuo. The crude product is purified by flash chromatography (95:5 CH2Cl2:MeOH) and its hydrochloride salt is prepared by reaction in acetone with the appropriate amount of ethereal HCl giving, after recrystallisation from ether, 1.1 g pure product (70%) as white crystals.
WORKUP
后处理
- temperatureto cool to rt overnight
- washthe organic phase is washed with water
- customdried
- concentrationconcentrated in vacuo
- customThe crude product is purified by flash chromatography (95:5 CH2Cl2:MeOH) and its hydrochloride salt
- customis prepared by reaction in acetone with the appropriate amount of ethereal HCl giving
- customafter recrystallisation from ether, 1.1 g pure product (70%) as white crystals