تفاعل #84256

ord-d2c13d02df2b4c4ea368ee52598af671

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAfter completion of the reaction
  2. 2
    استخلاصextracted with ethyl acetate (100 ml×1)
  3. 3
    غسيلthe resulting organic layer was washed with water (50 ml×1)
  4. 4
    تجفيفdried over saturated aqueous sodium chloride
  5. 5
    أخرىanhydrous sodium sulfate, and the solvent was evaporated under reduced pressure
  6. 6
    غسيلThe resulting residue was washed with 10 ml of diisopropyl ether

الإجراء التجريبي

To 3.00 g of 2-bromo-1-(3,5-dichloropyridin-2-yl)ethanone-O-ethyloxime in 20 ml of N,N-dimethylformamide, 2.32 g of potassium phthalimide was added, and the mixture was stirred at room temperature for 12 hours. After completion of the reaction, the reaction mixture was mixed with 50 ml of water and extracted with ethyl acetate (100 ml×1), the resulting organic layer was washed with water (50 ml×1) and dried over saturated aqueous sodium chloride and then anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The resulting residue was washed with 10 ml of diisopropyl ether to obtain 3.08 g of the desired product as white crystals. m.p.: 99.0 to 101.0° C.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09434684B2uspto-grants-2016_09