반응 #4335

ord-4c54e3751d4842d7a5094d5ea6aa2e59

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타An impurity is precipitated
  2. 2
    workup.ADDITIONby adding hydrochloric acid
  3. 3
    기타is removed by filtration
  4. 4
    기타The expected product precipitates
  5. 5
    여과After filtration
  6. 6
    기타drying
  7. 7
    기타it is purified as its hydrochloride
  8. 8
    기타before being recrystallized from alcohol

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04725283uspto-grants-1988_02