تفاعل #651851

ord-f1b52e810b6d4133a21517e0498647eb

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed for 5.5 hours
  2. 2
    workup.DISTILLATIONDiethylamine was distilled away under reduced pressure
  3. 3
    استخلاصthe residue was extracted with diethylether
  4. 4
    غسيلthe extract was washed with water
  5. 5
    workup.DISTILLATIONFrom the extract, diethylether was distilled away
  6. 6
    أخرىthe residue was purified by column chromatography (elution liquid: heptane-ethyl acetate)

الإجراء التجريبي

The mixture of 2-fluoro-4-iodotoluene (0.05 mol), 3-methyl-3-hydroxy-1-butyne (0.06 mol), tetrakis (triphenylphosphonium) palladium (0) 0.35 g, copper iodide 50 mg, and diethylamine 100 ml was refluxed for 5.5 hours. Diethylamine was distilled away under reduced pressure, the residue was extracted with diethylether, and the extract was washed with water. From the extract, diethylether was distilled away, the residue was purified by column chromatography (elution liquid: heptane-ethyl acetate) to obtain colorless oily 2-fluoro-4-(3-methyl-3-hydroxy-1-butynyl)toluene (0.035 mol).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06168728Auspto-grants-2001_01