تفاعل #60234

ord-9f1019e9f08e4c20928a76146f953959

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
60°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONCharged
  2. 2
    أخرىwas elevated up to 90° C.
  3. 3
    درجة الحرارةthe mixture was heated for 3 hours
  4. 4
    workup.STIRRINGwhile stirring
  5. 5
    workup.WAITThe reaction solution was left
  6. 6
    درجة الحرارةcooling down to room temperature
  7. 7
    أخرىThe precipitate formed
  8. 8
    ترشيحwas filtered
  9. 9
    غسيلwashed with ethanol and water
  10. 10
    أخرىThe solid matter thus obtained
  11. 11
    أخرىwas recrystallized from ethanol

الإجراء التجريبي

Charged were 2-bromofluorene 25.0 g, iodine 11.5 g, orthoperiodic acid 4.88 g, acetic acid 150 ml, conc. sulfuric acid 3 ml and water 10 ml, and the mixture was heated at 60° C. for 30 minutes while stirring. Further, the temperature was elevated up to 90° C., and the mixture was heated for 3 hours while stirring. The reaction solution was left cooling down to room temperature and poured into 500 ml of water. The precipitate formed was filtered and washed with ethanol and water. The solid matter thus obtained was recrystallized from ethanol to obtain 26.5 g of yellow crystal of 2-bromo-7-iodofluorene.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07425654B2uspto-grants-2008_09