تفاعل #44368

معادلة التفاعل

4-bromo-2-chlorobenzoic acid

5-chloro-2-methoxybenzoic acid

sodium carbonate

dioxan

→

sub-title compound

المردود 79.2%

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

المردود 79.2%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated
2. 2
   درجة الحرارةat reflux for 16 h
3. 3
   ترشيحfiltered (hyflo)
4. 4
   تركيزThe 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
   أخرىThe aqueous layer was separated
8. 8
   استخلاصextracted with EtOAc
9. 9
   تجفيفdried (MgSO4)
10. 10
    أخرىevaporated in vacuo

الإجراء التجريبي

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

المصدر