تفاعل #1857336

ord-3973910c6c67487ba60629d62f9c0794

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةby refluxing for 18 hours and 20 minutes
  2. 2
    أخرىAfter the reaction
  3. 3
    درجة الحرارةthe reaction mixture was cooled on an ice water bath
  4. 4
    أخرىto precipitate a crystal
  5. 5
    ترشيحThe crystal was recovered by filtration
  6. 6
    أخرىpurified by silica gel column chromatography (eluent: toluene)
  7. 7
    أخرىfollowed by recrystallization from a mixture solvent (acetone/methanol)

الإجراء التجريبي

0.80 g (2.59 mM) of 2-octyl-5-amidinoindan hydrochloride, 0.30 g (5.55 mM) of sodium methylate, 0.62 g (2.73 mM) of α-octyloxy-β-dimethylaminoacrolein and 12 ml of methanol were placed in a 30 ml-round bottomed flask, followed by refluxing for 18 hours and 20 minutes under stirring. After the reaction, the reaction mixture was cooled on an ice water bath to precipitate a crystal. The crystal was recovered by filtration and purified by silica gel column chromatography (eluent: toluene), followed by recrystallization from a mixture solvent (acetone/methanol) to obtain 0.57 g of 2-octyl-5-(5-octylpyrimidine-2-yl) indan (Yield: 50.4%). ##STR133##

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05385692uspto-grants-1995_01