반응 #456832
ord-273d7e61afd3408f82c30d9f7e75dba0
반응 방정식
2-chlorobenzonitrile
p-tolueneboronic acid
sodium carbonate
TPPTS H2O
→
2-cyano-4'-methylbiphenyl
수율 84.6%
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타the phases were separated
- 2세척The aqueous phase was washed with 50 ml of toluene
- 3세척The combined organic phases were washed with 20 ml of water
- 4건조subsequently dried over sodium sulfate
- 5기타Crystallization 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., 19.3 mg of palladium chloride, 17.9 mg of sodium acetate and 0.55 ml of TPPTS/H2O solution (0.6 molar) in 2.5 ml of DMSO were 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.