反応 #1503

ord-c2c590b87f0c4656985c4433af338c9a

試薬

なし

溶媒

反応条件

温度
125°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他equipped with a distillation head
  2. 2
    workup.ADDITIONDuring the course of the addition
  3. 3
    その他reached 140° C
  4. 4
    その他removed by distillation
  5. 5
    workup.ADDITIONit was poured into an aluminum pan
  6. 6
    温度to cool to ambient temperature
  7. 7
    その他to provide 468 g of crude product
  8. 8
    その他This material was recrystallized from methanol (1.9 L)

実験手順

Lactic acid (441 g; 4.90 moles) was placed in a reaction flask equipped with a distillation head. Under a nitrogen atmosphere, ethylene diamine (147 g; 2.45 moles) was slowly added with stirring to the reaction flask. During the course of the addition, the reaction mixture turned a deep orange and the temperature reached 140° C. The reaction mixture was then heated at 150° C. overnight with the water being removed by distillation. The reaction mixture was allowed to cool to 125° C. then it was poured into an aluminum pan and allowed to cool to ambient temperature. to provide 468 g of crude product. This material was recrystallized from methanol (1.9 L) to provide N,N'-1,2-ethanediylbislactamide, m.p. 188° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05725841uspto-grants-1998_03