تفاعل #1478574

ord-16c0fd29e0ed49c7ae84da016654edbe

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas refluxed for 42 hours
  2. 2
    ترشيحThe resulting mixture was filtered while hot and
  3. 3
    درجة الحرارةto cool
  4. 4
    ترشيحthe crystals were filtered off by suction
  5. 5
    غسيلwashed with absolute ethanol
  6. 6
    أخرىAfter drying
  7. 7
    أخرى87.9 g of crude product were obtained
  8. 8
    أخرىAfter two recrystallizations from acetonitrile

الإجراء التجريبي

A mixture of p-nitroaniline (55.2 g, 0.4 mol), calcium carbonate (80 g) and chloroacetamide (149.6 g, 1.6 mol) in 350 ml of water/ethanol (1/1) was refluxed for 42 hours. The resulting mixture was filtered while hot and allowed to cool, and the crystals were filtered off by suction, reslurried in water and then washed with absolute ethanol. After drying, 87.9 g of crude product were obtained. After two recrystallizations from acetonitrile, 45.3 g of pure product were obtained (melting point=178° C.).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07338536B2uspto-grants-2008_03