تفاعل #347284

ord-827e9f867bd341fb83dc1d0d03ac2252

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    استخلاصthe mixture was extracted with dichloromethane three times
  2. 2
    تجفيفdried over anhydrous sodium sulfate
  3. 3
    تركيزThe organic layer was concentrated
  4. 4
    أخرىthe residue was crystallized from ethyl acetate

الإجراء التجريبي

5.0 g of 3-nitro-4-chlorobenzaldehyde, 5.6 g of 3,4,5-trimethoxyphenylacetonitrile, 1.3 g of sodium hydroxide and 500 mg of trioctylmethylammonium chloride were dissolved in 10 ml of water and 50 ml of dichloromethane. The mixture was stirred vigorously for 3 hours at room temperature. The ice water was added to the mixture and the mixture was extracted with dichloromethane three times and dried over anhydrous sodium sulfate. The organic layer was concentrated and the residue was crystallized from ethyl acetate to give 4.9 g of the intended compound. The yield was 48.5%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05525632uspto-grants-1996_06