반응 #500802

반응 방정식

trisodiumphosphate dodecahydrate

4-bromo-2,6-difluoro-aniline

p-n-propylphenyl boronic acid

→

4′-n-propyl-3,5-difluoro-biphenyl-4-ylamine

수율 99.5%

용매

water

반응 조건

후처리

1. 1
   workup.ADDITION804 604) were added
2. 2
   workup.ADDITIONwere added
3. 3
   workup.DISSOLUTIONdissolved in 600 ml
4. 4
   기타dried tetrahydrafurane (Merck KGaA, Art. No.108 107)
5. 5
   workup.ADDITIONwas added dropwise
6. 6
   온도The reaction mixture was heated 6 hours
7. 7
   온도under reflux
8. 8
   기타The organic layer was separated
9. 9
   건조dried over Na2SO4
10. 10
    기타evaporated

실험 절차

348 g trisodiumphosphate dodecahydrate (Merck KGaA, Art. No.106 578) were dissolved in 500 ml of distilled water. Then 8.563 g bis(triphenylphosphine) palladium (Merck KGaA, Art. No. 804 174) and 0.611 g hydaziniumhydroxide (Merck KGaA, Art. No. 804 604) were added. The suspension was stirred for 5 minutes. Then, 126.886 g 4-bromo-2,6-difluoro-aniline, prepared in house, were added. Next 100 g of the p-n-propylphenyl boronic acid, prepared as described above, dissolved in 600 ml dried tetrahydrafurane (Merck KGaA, Art. No.108 107) was added dropwise. The reaction mixture was heated 6 hours under reflux. The organic layer was separated, dried over Na2SO4 and it's solvent evaporated. The isolated crude product (150 g of 4′-n-propyl-3,5-difluoro-biphenyl-4-ylamine was used for the next step of the reaction without further purificatoin.

출처