تفاعل #4468

ord-735fc3dbd8da40b9ad499f1ee9ee5a7e

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed for about 4 hours
  2. 2
    ترشيحfiltered
  3. 3
    تركيزthe filtrate was concentrated
  4. 4
    workup.DISSOLUTIONdissolved in ether
  5. 5
    غسيلThe ether solution was washed thoroughly with lN NaOH solution, water and brine
  6. 6
    تجفيفAfter drying the ether solution over anhydrous magnesium sulfate
  7. 7
    ترشيحfiltering off the drying agent
  8. 8
    أخرىthe solvent was evaporated off
  9. 9
    أخرىto leave the crude product which
  10. 10
    أخرىwas crystallized from hexane and ether

الإجراء التجريبي

A mixture of 2-chloromethyl quinoline (0.05 mol), phenol (0.055 mol), finely powdered potassium carbonate (0.055 mol), cesium carbonate (0.005 mol) and sodium iodide (0.0025 mol) in acetone was refluxed for about 4 hours. The reaction mixture was cooled to room temperature and filtered and the filtrate was concentrated and dissolved in ether. The ether solution was washed thoroughly with lN NaOH solution, water and brine. After drying the ether solution over anhydrous magnesium sulfate, and filtering off the drying agent, the solvent was evaporated off to leave the crude product which was crystallized from hexane and ether to yield the desired compound as a light yellow solid, m.p. 79.5°-80.5° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04725619uspto-grants-1988_02