تفاعل #4335

ord-4c54e3751d4842d7a5094d5ea6aa2e59

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAn impurity is precipitated
  2. 2
    workup.ADDITIONby adding hydrochloric acid
  3. 3
    أخرىis removed by filtration
  4. 4
    أخرىThe expected product precipitates
  5. 5
    ترشيحAfter filtration
  6. 6
    أخرىdrying
  7. 7
    أخرىit is purified as its hydrochloride
  8. 8
    أخرىbefore being recrystallized from alcohol

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US04725283uspto-grants-1988_02