HRID612032
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturewas refluxed for 1.5 hr
- customExcess reagent was removed at reduced pressure
- additionThe residue was mixed with ice cold dilute sodium hydroxide and ethyl acetate
- extractionThe mixture was extracted with a combination of ethyl acetate and tetrahydrofuran
- washThe combined extracts were washed with a saturated solution of sodium bicarbonate
- dry with materialdried over magnesium sulfate
- filtrationfilter through a short column of silica gel
- customSolvents were removed