تفاعل #1846

ord-f12406699295447fa245b2a1d83d7703

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
20°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux for 15 min
  2. 2
    workup.STIRRINGstirring
  3. 3
    أخرىAfter an exothermic reaction
  4. 4
    workup.STIRRINGstirring
  5. 5
    أخرىwas accompanied by a rise in temperature to 35° C
  6. 6
    درجة الحرارةThe mixture was cooled to 20° C.
  7. 7
    درجة الحرارةwith cooling
  8. 8
    workup.STIRRINGStirring
  9. 9
    workup.ADDITIONafter the addition

الإجراء التجريبي

Magnesium (36 g, 1.5 mol), iodine (a few crystals) and THF (1 L) were heated under nitrogen, with stirring, at reflux for 15 min. The mixture was cooled to 20° C., stirring stopped, and 1,2-dibromoethane (2.5 ml) added. After an exothermic reaction was observed (a few min) stirring was restarted which was accompanied by a rise in temperature to 35° C. The mixture was cooled to 20° C. and 4-bromoanisole slowly added over 1 h at 14°-18° C. with cooling. Stirring was continued for 10 min after the addition was complete.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05726315uspto-grants-1998_03