تفاعل #353600

ord-72eec48bc8f34d2287f3a88072a82324

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwas added dropwise to the mixture under ice cooling
  2. 2
    workup.ADDITIONwas added
  3. 3
    غسيلby washing twice with water (100 ml)
  4. 4
    تجفيفThe ether layer was dried over anhydrous magnesium sulfate
  5. 5
    تركيزconcentrated under reduced pressure
  6. 6
    أخرىthe resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane)

الإجراء التجريبي

To α-hydroxyimino-2-phenoxyphenylacetonitrile (a mixture of E- and Z-isomers) (1.19 9, 0.005 mole) were added dried dimethylformamide (10 ml) and potassium carbonate 0.90 g, 0.0065 mole), and dimethylsulfate (0.76 g, 0.006 mole) was added dropwise to the mixture under ice cooling, followed by stirring at room temperature for 1.5 hours. After completion of the reaction, ether (150 ml) was added, followed by washing twice with water (100 ml). The ether layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure, and then the resulting residue was purified by silica gel chromatography (ethyl acetate/n-hexane) to obtain α-methoxyimino-2-phenoxyphenylacetonitrile (1.13 g, yield: 89.6%) as a colorless oil.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05650539uspto-grants-1997_07