HRID2240284

反应详情

EQUATION

反应方程式

HRID 2240284 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

To a stirred solution of 2-ethyl-1-piperidin-4-yl-1H-benzimidazole (0.6 g) and (3-chloropropyl)-(4-fluorophenyl)amine (0.4 g) in DMF (7 ml) was added K2CO3 (1.1 g) and KI (0.1 g). The mixture was heated at 100° C. for 2 h, and then allowed to cool to rt. Water (50 ml) was added and the mixture extracted with ethyl acetate (80 ml), and the organic layer separated and washed with water. This was further dried and concentrated in vacuo. The oil was purified by flash chromatography (95:5 DCM:MeOH), and the solid recrystallised from ether to yield 0.3 g of the title compound as colourless crystals. Mp. 121-124° C.

WORKUP

后处理

  1. temperatureto cool to rt
  2. extractionthe mixture extracted with ethyl acetate (80 ml)
  3. customthe organic layer separated
  4. washwashed with water
  5. customThis was further dried
  6. concentrationconcentrated in vacuo
  7. customThe oil was purified by flash chromatography (95:5 DCM:MeOH)
  8. customthe solid recrystallised from ether