تفاعل #1379890

ord-e796985f790a46e48b1f769398221cab

الكواشف

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المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةat reflux for 48 h
  2. 2
    درجة الحرارةto cool to ambient,
  3. 3
    استخلاصthe filtrate extracted with diethyl ether (3×100 ml)
  4. 4
    أخرىThe precipitate which formed
  5. 5
    ترشيحwas collected by filtration
  6. 6
    غسيلwashed first with water (200 ml)
  7. 7
    تجفيفwith acetone (200 ml) before being dried

الإجراء التجريبي

A mixture of 5-aminoquinoline (9.9 g, 0.069 mol) and crotonic acid (8.9 g, 0.103 mol) in toluene (35 ml) was stirred at reflux for 48 h. The reaction mixture was allowed to cool to ambient, added to water (500 ml) and the pH adjusted to 9 to 10 by the addition of 2N sodium hydroxide. The reaction mixture was screened and the filtrate extracted with diethyl ether (3×100 ml). The pH of the aqueous layer was first adjusted to pH2 with concentrated HCl and then to pH7 with calcium hydroxide. The precipitate which formed was collected by filtration, washed first with water (200 ml) and then with acetone (200 ml) before being dried to give 8.1 g of a cream solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07238228B2uspto-grants-2007_07