HRID2356387

反应详情

EQUATION

反应方程式

HRID 2356387 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

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

  1. temperatureto cool to rt overnight
  2. washthe organic phase is washed with water
  3. customdried
  4. concentrationconcentrated in vacuo
  5. customThe crude product is purified by flash chromatography (95:5 CH2Cl2:MeOH) and its hydrochloride salt
  6. customis prepared by reaction in acetone with the appropriate amount of ethereal HCl giving
  7. customafter recrystallisation from ether, 1.1 g pure product (70%) as white crystals