반응 #44368

반응 방정식

4-bromo-2-chlorobenzoic acid

5-chloro-2-methoxybenzoic acid

sodium carbonate

dioxan

→

sub-title compound

수율 79.2%

3,5′-dichloro-2′-methoxy-[1,1′-biphenyl]-4-carboxylic acid

수율 79.2%

용매

methanol

반응 조건

후처리

1. 1
   온도heated
2. 2
   온도at reflux for 16 h
3. 3
   여과filtered (hyflo)
4. 4
   농축The filtrate was concentrated in vacuo
5. 5
   workup.DISSOLUTIONdissolved in ethyl acetate
6. 6
   workup.ADDITIONThe suspension was made basic by addition of dilute NaOH
7. 7
   기타The aqueous layer was separated
8. 8
   추출extracted with EtOAc
9. 9
   건조dried (MgSO4)
10. 10
    기타evaporated in vacuo

실험 절차

4-bromo-2-chlorobenzoic acid (0.4 g), 5-chloro-2-methoxybenzoic acid (0.4 g), Pd(dppf)Cl2 (0.12 g), sodium carbonate (0.9 g), dioxan (15 ml) and methanol (5 ml) were charged to a flask and heated at reflux for 16 h. Cooled to room temp and filtered (hyflo). The filtrate was concentrated in vacuo, then dissolved in ethyl acetate. The suspension was made basic by addition of dilute NaOH. The aqueous layer was separated and acidified using 2M HCl, extracted with EtOAc, dried (MgSO4) and evaporated in vacuo to give the sub-title compound Yield 0.4 g

출처