تفاعل #1149061

ord-d7a6da0d23cd412b8dd5363bbc21bb3f

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةcooling
  2. 2
    أخرىA half amount of the solvent was evaporated under reduced pressure
  3. 3
    workup.ADDITIONthe residue was diluted with ethyl acetate
  4. 4
    غسيلwashed successively with water, 1N aqueous sodium hydroxide solution, water and saturated brine
  5. 5
    تجفيفdried over magnesium sulfate
  6. 6
    أخرىThe solvent was evaporated
  7. 7
    غسيلthe obtained solid was washed with isopropyl ether

الإجراء التجريبي

To a solution (800 mL) of diisopropylamine (112 mL) and triethylamine (112 mL) in THF was added dropwise a solution (400 mL) of 6-bromo-2-naphthoyl chloride in THF under ice-cooling. The mixture was stirred at room temperature for 1 hr. A half amount of the solvent was evaporated under reduced pressure, and the residue was diluted with ethyl acetate, washed successively with water, 1N aqueous sodium hydroxide solution, water and saturated brine and dried over magnesium sulfate. The solvent was evaporated and the obtained solid was washed with isopropyl ether to give the title compound (117 g) as colorless flakes.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06960586B2uspto-grants-2005_11