تفاعل #49366

ord-07fff94954834be4b0ddba67b532291f

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooled
  2. 2
    ترشيحfiltered
  3. 3
    استخلاصThe filtrate was extracted with ethyl acetate
  4. 4
    تجفيفThe organic layer was dried over anhydrous sodium sulfate
  5. 5
    أخرىThe solvent was evaporated under reduced pressure
  6. 6
    أخرىThe residue was purified by slurry

الإجراء التجريبي

3-Amino-6-bromophthalimide (3.10 g, 12.9 mmol) was dissolved in THF (240 mL), and the solution was added with diisobutylaluminiumhydride (0.94 mol/L, 68.6 mL, 64.5 mmol) by drops at −78° C. for 25 minutes, then the reaction mixture was warmed to room temperature, followed by stirring for 1.5 hours. Then, the reaction mixture was ice-cooled, added with water and filtered using Celite. The filtrate was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by slurry using chloroform to obtain 7-amino-4-bromo-3-hydroxyisoindolinone (2.26 g, yield 72%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07745641B2uspto-grants-2010_06