تفاعل #49540

ord-8d965707b7cb44bcb339cf9e8020bc5b

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvent was evaporated under reduced pressure
  2. 2
    workup.DISSOLUTIONthe residue was dissolved in acetonitrile (5 mL)
  3. 3
    workup.ADDITIONThe solution was added with 1 mol/L hydrochloric acid (5 mL)
  4. 4
    workup.STIRRINGstirred at room temperature for 1 hour
  5. 5
    ترشيحThe precipitated solid was collected by filtration
  6. 6
    غسيلwashed with water
  7. 7
    أخرىby drying under reduced pressure

الإجراء التجريبي

4-Methoxymethoxy-5-dimethoxymethyl-3-hydroxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (490 mg, 0.929 mmol) was dissolved in methanol (10 mL), and the solution was treated with 10% hydrogen chloride-methanol solution (5 mL), followed by stirring at room temperature for 3 hours. The solvent was evaporated under reduced pressure and the residue was dissolved in acetonitrile (5 mL). The solution was added with 1 mol/L hydrochloric acid (5 mL) and stirred at room temperature for 1 hour. The precipitated solid was collected by filtration and washed with water, followed by drying under reduced pressure to obtain 4-hydroxy-5-formyl-3-methoxy-7-iodo-2-(1-methyl-1-phenylethyl)isoindolinone (329 mg, yield 79%).

المصدر

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