تفاعل #1764734

ord-57f060bf6bad401bb1dd0b76338e7986

المذيبات

ظروف التفاعل

درجة الحرارة
50°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةthe reaction was heated at 50° C. overnight
  2. 2
    أخرىMost of the solvent was removed on a rotary evaporator
  3. 3
    أخرىThe solid residue was triturated with 20% ethyl acetate in hexanes
  4. 4
    ترشيحfiltered
  5. 5
    أخرىdried

الإجراء التجريبي

3-Bromo-phenylamine (10.0 g, 58.1 mmol) and 3,3-dimethyl-dihydro-furan-2,5-dione (8.2 g, 63.9 mmol) were suspended in 387 ml of methylene chloride and heated at 50° C. for 3 hours. Carbonyldiimidazole (11.3 g, 69.7 mmol) was added in portions and the reaction was heated at 50° C. overnight. Most of the solvent was removed on a rotary evaporator. The solid residue was triturated with 20% ethyl acetate in hexanes, filtered and dried to give 15 g (92%) of somewhat impure 1-(3-bromo-phenyl)-3,3-dimethyl-pyrrolidine-2,5-dione which was used without further purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08008298B2uspto-grants-2011_08