반응 #5639

반응 방정식

4,7-dichloroquinoline

4-fluorophenol

→

product

4-(4-Fluorophenoxy)-7-chloroquinoline

용매

xylene

반응 조건

후처리

1. 1
   기타To a 50 mL flask equipped with a condenser
2. 2
   기타drying tube
3. 3
   workup.ADDITIONwere added
4. 4
   온도The reaction mixure was heated
5. 5
   온도to reflux
6. 6
   온도maintained at that temperature for 18 hr
7. 7
   여과The reaction mixture was filtered hot
8. 8
   기타to remove the polymer
9. 9
   온도After cooling
10. 10
    세척the filtrate was washed with 50 mL of 5N NaOH
11. 11
    추출The caustic layer was extracted with 2×25 mL of diethyl ether
12. 12
    건조dried over Na2SO4
13. 13
    기타Removal of the solvent

실험 절차

To a 50 mL flask equipped with a condenser, drying tube and thermometer, was added 1.98 g (0.01 moles) of 4,7-dichloroquinoline, 1.07 g (0.0015 moles) of polyDMAP™and 20 mL of xylene. The mixture was stirred to reswell the polymer and 1.57 g (0.0014 moles) of 4-fluorophenol were added. The reaction mixure was heated to reflux and maintained at that temperature for 18 hr. The reaction mixture was filtered hot to remove the polymer. After cooling, the filtrate was washed with 50 mL of 5N NaOH. The caustic layer was extracted with 2×25 mL of diethyl ether. The xylene and the ether layers were combined and dried over Na2SO4. Removal of the solvent provided 2.36 g (86 percent yield) of product, mp=89°-91° C.

출처