반응 #456820

반응 방정식

2-chlorobenzonitrile

p-tolueneboronic acid

sodium carbonate

TPPTS H2O

→

2-cyano-4'-methylbiphenyl

수율 84.6%

용매

p-xylene

triethanolamine

water

DMSO

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   기타the phases were separated
3. 3
   세척The aqueous phase was washed with 50 ml of toluene
4. 4
   세척The combined organic phases were washed with 20 ml of water
5. 5
   건조subsequently dried over sodium sulfate
6. 6
   기타Crystallization from n-heptane

실험 절차

15 g of 2-chlorobenzonitrile, 14.8 g of p-tolueneboronic acid and 28.9 g of sodium carbonate in 50 ml of p-xylene, 40 ml of triethanolamine and 10 ml of water were heated to 120° C. At 80° C., a mixture of 38.66 g of palladium(II) chloride and 1.1 ml of TPPTS/H2O solution (0.6 molar) in 2.5 ml of DMSO was added. After the reaction was complete, the phases were separated. The aqueous phase was washed with 50 ml of toluene. The combined organic phases were washed with 20 ml of water and subsequently dried over sodium sulfate. Crystallization from n-heptane gave 17.8 g of 2-cyano-4'-methylbiphenyl.

출처