تفاعل #64040

ord-ea4ac235a9be4f3da8afc55c10b4281d

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىthe ethanol was removed by evaporation under reduced pressure
  2. 2
    workup.ADDITIONThe residue was treated with dichloromethane
  3. 3
    غسيلthe organic phase was washed twice with water
  4. 4
    تجفيفdried over anhydrous sodium sulfate
  5. 5
    أخرىThe solvent was removed by evaporation under reduced pressure

الإجراء التجريبي

Ethoxyamine hydrochloride (0.26 g; 2.7 mmole) and then sodium hydroxide (0.11 g; 2.7 mmole) were added to a solution of 3-hydroxy-5-(2,4,6-trimethyl-3-nitrophenyl)-2-propionylcyclohex-2-en-1-one (0.6 g; 1.8 mmole) in absolute ethanol (150 ml). The mixture was stirred at room temperature for a period of 18 hours and then the ethanol was removed by evaporation under reduced pressure. The residue was treated with dichloromethane and the organic phase was washed twice with water and dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure to give the product, 2-[1-(ethoxyimino)propyl]-3-hydroxy-5-(2,4,6-trimethyl-3-nitrophenyl)cyclohex-2-en-1one (0.56 g; 83.2%) as a pale yellow oil. The product was characterized by proton nuclear magnetic resonance spectroscopy and the spectroscopic data is recorded in Table 5, Example 37.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04767879uspto-grants-1988_08