HRID1934954
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 125 °C
PROCEDURE
实验过程
A mixture of 1 g (2.38 mmol) of 4-(4-Chloro-2-fluoro-phenylamino)-7-(3-chloro-propoxy)-6-methoxy-quinoline-3-carbonitrile and 0.07 g of sodium iodide in 17.85 ml of 2M dimethylamine in tetrahydrofuran was placed in a sealed tube and heated to 125° C. for 3.5 hr. The solvent was removed and the residue was mixed with warm ethyl acetate and saturated sodium bicarbonate solution. The organic layer was separated and dried over magnesium sulfate. Solvent was removed and ether was added. One standing, the crystals were deposited giving 0.93 g of the title compound as a white solid: mass spectrum (electrospray, m/e) M+H 428.9.
WORKUP
后处理
- customwas placed in a sealed tube
- customThe solvent was removed
- additionthe residue was mixed with warm ethyl acetate and saturated sodium bicarbonate solution
- customThe organic layer was separated
- dry with materialdried over magnesium sulfate
- customSolvent was removed
- additionether was added