تفاعل #53586

ord-122d9f4f153a4bfe8647dcb016a5c1e7

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةunder reflux
  2. 2
    درجة الحرارةwith heating for 2 hours
  3. 3
    workup.ADDITIONThe reaction mixture was poured into ice-cold water
  4. 4
    استخلاصextracted with toluene
  5. 5
    غسيلThe toluene layer was washed with water twice
  6. 6
    تجفيفdried over anhydrous magnesium sulfate
  7. 7
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

الإجراء التجريبي

1.0 g (5.2 mmol) of 2,4-dichlorophenylboronic acid, 1.1 g (5.5 mmol) of 4-bromo-2-fluorobenzonitrile, 1.6 g (15.0 mmol) of sodium carbonate and 0.8 g (0.7 mmol) of tetrakis(triphenylphosphine) palladium were added to a solvent mixture of 50 ml of toluene, 25 ml of ethanol and 25 ml of water, and the reaction was carried out under reflux with heating for 2 hours. The reaction mixture was poured into ice-cold water and extracted with toluene. The toluene layer was washed with water twice and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 1.3 g of 2-fluoro-4-(2,4-dichlorophenyl)benzonitrile (yield 93.0%), which was used in Example 8 (1) as the starting material.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06858639B2uspto-grants-2005_02