تفاعل #1610128

ord-4f45814b3b0e4302954abd2bf57c1043

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
70°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىA 100 mL 3-neck flask was equipped with a magnetic stirrer, a reflux condenser
  2. 2
    workup.DISSOLUTIONhad dissolved (about 2 hours)
  3. 3
    أخرىto about 80° C.
  4. 4
    أخرىsolids separated
  5. 5
    workup.STIRRINGAfter stirring at room temperature for about 2 hours
  6. 6
    ترشيحthe mixture was filtered
  7. 7
    غسيلThe solids were washed on the
  8. 8
    ترشيحfilter with a little water
  9. 9
    أخرىdried

الإجراء التجريبي

A 100 mL 3-neck flask was equipped with a magnetic stirrer, a reflux condenser, a nitrogen blanket, and a heating mantle with a temperature controller and a thermocouple. The flask was charged with o-phenylphenol (3.42 grams, 0.02 moles), with KOH pellets (1.37 grams, 0.02 moles, 85%), and with 15 mL of DMSO. The mixture was stirred at 100° C. under nitrogen until all of the KOH had dissolved (about 2 hours). The dark solution was cooled to 70° C., then the 1-chlorohexadecane (5.22 grams, 0.02 moles) was then added all at once. An exotherm to about 80° C. was observed. The reaction mixture was then stirred at 75° C. for about 7.5 hours, then it was poured into about 500 mL of water; solids separated. After stirring at room temperature for about 2 hours, the mixture was filtered. The solids were washed on the filter with a little water, then they were air dried to give 7.58 grams of waxy white solid. The yield was 96%; mp=35-37° C. Structure was confirmed by IR, GC/MS, and 1H- and 13C-NMR analyses.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09079838B2uspto-grants-2015_07