反应详情

温度

125 °C

A mixture of 0.8 g (1.83 mmol) of 4-(4-chloro-2-fluoro-5-hydroxy-phenylamino)-7-(3-chloro-propoxy)-6-methoxy-quinoline-3-carbonitrile and 0.055 g of sodium iodide in 15.6 ml of 2M dimethylamine in tetrahydrofuran was placed in a sealed tube and heated to 125° C. for 2.5 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 the residue was treated with with ethyl acetate-ether depositing a solid and giving 0.51 g of the title compound as a off-white solid: mass spectrum (electrospray, m/e) M+H 445.0; (M+2H)+2 243.4.

1. customwas placed in a sealed tube
2. customThe solvent was removed
3. additionthe residue was mixed with warm ethyl acetate and saturated sodium bicarbonate solution
4. customThe organic layer was separated
5. dry with materialdried over magnesium sulfate
6. customSolvent was removed
7. additionthe residue was treated with with ethyl acetate-ether depositing a solid