تفاعل #160651

ord-b4ff055354a04820a90d661e9004a69b

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةunder reflux
  3. 3
    درجة الحرارةwith reflux condenser
  4. 4
    workup.STIRRINGThe formed suspension was stirred intensively by means of a mechanical stirrer until the initially increased temperature
  5. 5
    أخرىhad returned to room temperature
  6. 6
    ترشيحThe crystals present were then filtered off
  7. 7
    غسيلwashed thoroughly with water
  8. 8
    أخرىthe product recrystallized from a mixture of 1200 ml ethanol and 300 ml water
  9. 9
    أخرىAfter drying to constant weight in the vacuum
  10. 10
    أخرىdrying cupboard at 70-80° C

الإجراء التجريبي

A mixture of 73.3 g (0.6 mol) p-hydroxybenzaldehyde, 73.2 g (0.3 mol) 1,6-dibromohexane, 39.6 g (0.6 mol) potassium hydroxide and 240 ml dimethylformamide was heated under reflux, accompanied by stirring for 1 h, in a 500 ml three-necked flask with reflux condenser, internal thermometer and magnetic stirrer. After cooling the reaction mixture to room temperature, the obtained crystal slurry was placed in a 2-1 beaker containing 1 l of deionized water. The formed suspension was stirred intensively by means of a mechanical stirrer until the initially increased temperature had returned to room temperature. The crystals present were then filtered off, washed thoroughly with water and the product recrystallized from a mixture of 1200 ml ethanol and 300 ml water. After drying to constant weight in the vacuum drying cupboard at 70-80° C. 63.5 g (65% of the theoretical value) 1,6-bis(4-formylphenoxy)hexane (m.p.: 109.8-111.2° C.) was obtained in the form of white crystals.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08829067B2uspto-grants-2014_09