تفاعل #435905

ord-d6b0d115572c49eeb8bce110d6f0dab3

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthermal reflux for 2 hours under an argon atmosphere
  2. 2
    أخرىAfter the reaction
  3. 3
    أخرىa precipitate was removed through filtration
  4. 4
    غسيلwashed with water
  5. 5
    تجفيفby drying with magnesium sulfate
  6. 6
    workup.DISTILLATIONThe solvent was distilled off
  7. 7
    أخرىthe residue was then purified through silica gel column chromatography (hexane/ethyl acetate)

الإجراء التجريبي

In carbon tetrachloride (26 ml), 2,6-dimethylquinoline (manufactured by Tokyo Kasei Kogyo Co., Ltd.) (1.0398 g), N-bromosuccinimide (1.2353 g), and azobisisobutyronitrile (98.5 mg) were dissolved and then the whole was subjected to thermal reflux for 2 hours under an argon atmosphere. After the reaction, a precipitate was removed through filtration and then washed with water, followed by drying with magnesium sulfate. The solvent was distilled off and the residue was then purified through silica gel column chromatography (hexane/ethyl acetate), thereby obtaining the subject compound (427.3 mg) as a white solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07176227B2uspto-grants-2007_02