反応 #4335

ord-4c54e3751d4842d7a5094d5ea6aa2e59

反応方程式

NCCNc1cc(Cl)c(Cl)cc1[N+](=O)[O-]
4,5-dichloro-2-nitro-N-β-aminoethylaniline
NCCO
monoethanolamine
NCCNc1cc(NCCO)c(Cl)cc1[N+](=O)[O-]
2-chloro-5-β-aminoethylamino-4-nitro-N-(β-hydroxyethyl)aniline

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他An impurity is precipitated
  2. 2
    workup.ADDITIONby adding hydrochloric acid
  3. 3
    その他is removed by filtration
  4. 4
    その他The expected product precipitates
  5. 5
    ろ過After filtration
  6. 6
    その他drying
  7. 7
    その他it is purified as its hydrochloride
  8. 8
    その他before being recrystallized from alcohol

実験手順

0.04 mole (10 g) of 4,5-dichloro-2-nitro-N-β-aminoethylaniline prepared in the 1st stage is heated in 40 ml of monoethanolamine for 30 minutes to 100° C. The reaction mixture is diluted with 450 ml of iced water. An impurity is precipitated by adding hydrochloric acid and is removed by filtration. The filtrate is made alkaline with concentrated sodium hydroxide solution. The expected product precipitates. After filtration and drying, it is purified as its hydrochloride before being recrystallized from alcohol. It melts at 160° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04725283uspto-grants-1988_02