HRID612032

反应详情

EQUATION

反应方程式

HRID 612032 的结构方程式

PROCEDURE

实验过程

A mixture of 3.5 g (12 mmol) of 7-(3-chloro-propoxy)-4-hydroxy-6-methoxy-quinoline-3-carbonitrile and 28 ml of phosphorous oxychloride was refluxed for 1.5 hr. Excess reagent was removed at reduced pressure. The residue was mixed with ice cold dilute sodium hydroxide and ethyl acetate. The mixture was extracted with a combination of ethyl acetate and tetrahydrofuran. The combined extracts were washed with a saturated solution of sodium bicarbonate, dried over magnesium sulfate, and filter through a short column of silica gel. Solvents were removed giving 3.2 g of the title compound as a pink solid that is used with additional purification.

WORKUP

后处理

  1. temperaturewas refluxed for 1.5 hr
  2. customExcess reagent was removed at reduced pressure
  3. additionThe residue was mixed with ice cold dilute sodium hydroxide and ethyl acetate
  4. extractionThe mixture was extracted with a combination of ethyl acetate and tetrahydrofuran
  5. washThe combined extracts were washed with a saturated solution of sodium bicarbonate
  6. dry with materialdried over magnesium sulfate
  7. filtrationfilter through a short column of silica gel
  8. customSolvents were removed