تفاعل #51442

ord-26d3f179119941d39512cec2ecd01884

المذيبات

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىlowered to −78° C
  2. 2
    درجة الحرارةthe solution is warmed at room temperature
  3. 3
    أخرىAfter evaporation of the solvent
  4. 4
    workup.DISTILLATIONthe residue is distilled under vacuum

الإجراء التجريبي

To a solution of 19 ml (0.135 mole) of diisopropylamine in 125 ml of tetrahydrofuran (THF) cooled at −20° C. is added 80 ml of n-butyllithium (1.6 M in hexane). The temperature is raised to 0° C. for 5 minutes and lowered to −78° C. Then 25 g (0.129 mole) of 2,4-difluoro-bromobenzene is then added and the reaction is stirred at 65° C. for 2 hours. Then, 25 ml (0.164 mole) of hexachloroacetone is added and the solution is warmed at room temperature. After evaporation of the solvent, the residue is distilled under vacuum to give the desired product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06849740B2uspto-grants-2005_02