反应详情

温度

-5 °C

To a single-neck reaction flask (100 ml) were added 2-(1-(tert-butyloxycarbonyl)piperidin-4-ylidene)acetic acid (1 g) and anhydrous THF (20 ml). The mixture was stirred to dissolve and cooled to the temperature of −5° C. To the mixture were added isobutyl chloroformate (0.6 ml) and N-methylmorphine (0.5 ml). The resultant mixture was stirred for 20 min. 6-amino-4-(3-chloro-4-(pyridin-2-yl-methoxy) phenylamino)-7-(tetrahydrofuran-3-yl-oxy)quinolin-3-carbonitrile (2 g, 4.1 mmol) was dissolved in anhydrous pyridine (20 ml). The resulting solution was added into the reaction flask in an ice-water bath. After the reaction finished, the solvent was rotary-evaporated to dryness. To the residue were added chloroform and water. The solution was stood for separation. The chloroform layer was wash once with saturated saline solution, dried over anhydrous magnesium sulfate, filtered and rotary-evaporated to dryness to give a crude product. The product was recrystallized with ethanol.

1. dissolutionto dissolve
2. additionThe resulting solution was added into the reaction flask in an ice-water bath
3. customthe solvent was rotary-evaporated to dryness
4. additionTo the residue were added chloroform and water
5. customThe solution was stood for separation
6. washThe chloroform layer was wash once with saturated saline solution
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. customrotary-evaporated to dryness