反应 #1478574

ord-16c0fd29e0ed49c7ae84da016654edbe

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was refluxed for 42 hours
  2. 2
    过滤The resulting mixture was filtered while hot and
  3. 3
    温度to cool
  4. 4
    过滤the crystals were filtered off by suction
  5. 5
    洗涤washed with absolute ethanol
  6. 6
    其他After drying
  7. 7
    其他87.9 g of crude product were obtained
  8. 8
    其他After two recrystallizations from acetonitrile

实验过程

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.).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07338536B2uspto-grants-2008_03