反应详情

7.96 g of the crude product of 6-fluoroisatin were added to 55 mL of water followed by the addition of 16.2 g (6 equivalents) of KOH while cooling with ice and stirring for 30 minutes. 9.9 g (1.5 equivalents) of bromoacetophenone were dropped into the resultant suspension while holding the internal temperature of the reaction mixture at 20° C. to 25° C. followed by additionally stirring overnight at room temperature. After neutralizing with concentrated hydrochloric acid, the precipitated crystals were filtered out and washed with a small amount of water. After adequately drying the resulting crystals, 70 mL of nitrobenzene heated to 120° C. to 130° C. were added a little at a time followed by further stirring for 1 hour at 140° C. to 150° C. After cooling the reaction mixture to room temperature, the precipitated crystals were washed with chloroform to obtain 5.4 g of 7-fluoro-3-hydroxy-2-methylquinoline.

1. temperaturewhile cooling with ice
2. customat 20° C. to 25° C.
3. stirringby additionally stirring overnight at room temperature
4. filtrationthe precipitated crystals were filtered out
5. washwashed with a small amount of water
6. dry with materialAfter adequately drying the resulting crystals, 70 mL of nitrobenzene
7. temperatureheated to 120° C. to 130° C.
8. additionwere added a little at a time
9. stirringby further stirring for 1 hour at 140° C. to 150° C
10. washthe precipitated crystals were washed with chloroform