반응 #1478574

ord-16c0fd29e0ed49c7ae84da016654edbe

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도was refluxed for 42 hours
  2. 2
    여과The resulting mixture was filtered while hot and
  3. 3
    온도to cool
  4. 4
    여과the crystals were filtered off by suction
  5. 5
    세척washed with absolute ethanol
  6. 6
    기타After drying
  7. 7
    기타87.9 g of crude product were obtained
  8. 8
    기타After two recrystallizations from acetonitrile

실험 절차

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.).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07338536B2uspto-grants-2008_03