反应详情

温度

135 °C

8-amino-6-chloroquinoline (Step 1, 0.49 g) and bis(chloroethyl)amine hydrochloride (0.49 g) were dissolved in chlorobenzene (13 mL) and heated with vigorous stirring at 135° C. for 5 days. The reaction was cooled to room temperature, diluted with water and extracted with Et2O. The aqueous phase was made basic by addition of solid Na2CO3 and then extracted with Et2O. The combined organic layers were dried over anhydrous Na2SO4, filtered and concentrated on a rotary evaporator to give the desired compound (0.20 g) as a yellow semi-solid; MS (ES) m/z (relative intensity) 248 (M+H)+ (100).

1. temperatureheated
2. temperatureThe reaction was cooled to room temperature
3. extractionextracted with Et2O
4. additionThe aqueous phase was made basic by addition of solid Na2CO3
5. extractionextracted with Et2O
6. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
7. filtrationfiltered
8. concentrationconcentrated on a rotary evaporator