تفاعل #47816

ord-25ef1506204e440cafabec79ffa9cfc6

ظروف التفاعل

درجة الحرارة
150°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةby cooling
  2. 2
    غسيلThe resulting mixture was washed with saturated ammonium chloride
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    أخرىThe organic layer was separated
  5. 5
    تجفيفdried over anhydrous MgSO4
  6. 6
    تركيزconcentrated under a reduced pressure
  7. 7
    أخرىThe resulting residue was purified by flash chromatography (ethyl acetate:hexane=1:3)

الإجراء التجريبي

2-Bromo-3-phenyl-6-(3-phenyl-propoxy)-indene-1-one (1.0 g, 2.3 mmol) obtained in Step 2 was dissolved in N,N-dimethyl formamide (10 mL), copper(I) cyamide (617 mg, 6.9 mmol) was added thereto, and the mixture was stirred for 3 hrs at 150° C., followed by cooling. The resulting mixture was washed with saturated ammonium chloride and extracted with ethyl acetate. The organic layer was separated, dried over anhydrous MgSO4 and concentrated under a reduced pressure. The resulting residue was purified by flash chromatography (ethyl acetate:hexane=1:3) to obtain 700 mg of the titled compound (yield: 80%) as a red solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07745439B2uspto-grants-2010_06