HRID393652

反应详情

EQUATION

反应方程式

HRID 393652 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

1,3-Dihydroxybenzene (110 mg, 1 mmol) was added to a stirred suspension of sodium hydride (60 mg, 2 mmol) in DMF (10 ml) and the mixture was stirred for 30 minutes. 4-Chloro-6-cyano-7-(2-methoxyethoxy)quinoline hydrochloride (300 mg 1 mmol), (prepared as described for the starting material in Example 1), was added and the mixture was heated at 100° C. for 4 hours. The mixture was allowed to cool, was quenched with water and extracted with ethyl acetate (2×75 ml). The extracts were combined, washed with water (×2) and then brine and dried (MgSO4). The solvent was removed by evaporation and the residue was triturated with ethyl acetate/hexane, collected by filtration and dried to give 6-cyano-4-(3-hydroxyphenoxy)-7-(2-methoxyethoxy)quinoline (115 mg, 34%).

WORKUP

后处理

  1. additionwas added
  2. temperatureto cool
  3. customwas quenched with water
  4. extractionextracted with ethyl acetate (2×75 ml)
  5. washwashed with water (×2)
  6. dry with materialbrine and dried (MgSO4)
  7. customThe solvent was removed by evaporation
  8. customthe residue was triturated with ethyl acetate/hexane
  9. filtrationcollected by filtration
  10. customdried