تفاعل #1985941

ord-8a80e624349342b3b650619df4c01469

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
45°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGstirred at room temperature for 3 days
  2. 2
    ترشيحfiltered
  3. 3
    workup.DISSOLUTIONThe solid is dissolved in toluene
  4. 4
    غسيلthe solution washed with brine
  5. 5
    تجفيفdried over magnesium sulfate
  6. 6
    ترشيحfiltered
  7. 7
    تركيزconcentrated in vacuo
  8. 8
    أخرىThe residue is recrystallized twice from hexanes

الإجراء التجريبي

To a mixture of 4-acetoxy-3-methoxybenzaldehyde (75.7 g), anhydrous sodium acetate (76 g) and iodine (0.8 g) in acetic acid (300 ml) is added bromine (21 ml). The mixture is warmed to 45° C. for about 1 hour, then stirred stirred at room temperature for 3 days, poured into water (700 ml) and filtered. The solid is dissolved in toluene and the solution washed with brine, dried over magnesium sulfate, filtered and concentrated in vacuo. The residue is recrystallized twice from hexanes to give the desired product.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05571506uspto-grants-1996_11