تفاعل #65932

ord-8ffda47fa00c4b12a1a6271460898719

الكواشف

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المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe solution was refluxed for 1 hour
  2. 2
    استخلاصextracted with toluene
  3. 3
    تجفيفThe organic phase was dried with sodium sulfate
  4. 4
    أخرىevaporated to dryness
  5. 5
    أخرىThe residue was purified by flash chromatography on silica gel by elution with ethyl acetate/hexane 1:9

الإجراء التجريبي

3-Dipropylamino-5-aminochroman (Example 14; 0.60 g, 2.42 mmol) was dissolved in acetic acid (10 ml) and 2,5-dimethoxytetrahydrofuran (0.40 g, 3.0 mmol) was added. The solution was refluxed for 1 hour. The solution was neutralized with NaOH (aq.) and extracted with toluene. The organic phase was dried with sodium sulfate and evaporated to dryness. The residue was purified by flash chromatography on silica gel by elution with ethyl acetate/hexane 1:9 to give the title compound. 13C-NMR: 111.75 21.89 24.81 52.69 53.15 67.94 108.93 115.67 118.22 118.44 121.87 127.22 141.47 155.27.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05420151uspto-grants-1995_05