HRID1721688

反应详情

EQUATION

反应方程式

HRID 1721688 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 6-(quinol-2-ylmethoxy)nicotinic acid methyl ester (5.06 g, 17.2 mmol), prepared as in step 2, in methanol (100 ml) at room temperature with stirring was added. 1N NaOH (18.9 ml, 18.9 mmol). The resulting mixture was allowed to stir at room temperature for 14 hours. The mixture was then refluxed for 3 hours, cooled to room temperature and concentrated in vacuo. The residue was diluted with water and the aqueous layer was extracted with ethyl acetate. The aqueous layer was acidified to pH 3 with 10% citric acid to give a white precipitate. The precipitate was filtered and washed with water and diethyl ether. The solid was dried overnight at 80° C. under reuced pressure to give 4.46 g of 6-(2-quinolylmethoxy)nicotinic acid.

WORKUP

后处理

  1. additionwas added
  2. temperatureThe mixture was then refluxed for 3 hours
  3. temperaturecooled to room temperature
  4. concentrationconcentrated in vacuo
  5. additionThe residue was diluted with water
  6. extractionthe aqueous layer was extracted with ethyl acetate
  7. customto give a white precipitate
  8. filtrationThe precipitate was filtered
  9. washwashed with water and diethyl ether
  10. customThe solid was dried overnight at 80° C. under reuced pressure