반응 #4335
ord-4c54e3751d4842d7a5094d5ea6aa2e59
반응 방정식
4,5-dichloro-2-nitro-N-β-aminoethylaniline
monoethanolamine
→
2-chloro-5-β-aminoethylamino-4-nitro-N-(β-hydroxyethyl)aniline
용매
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1기타An impurity is precipitated
- 2workup.ADDITIONby adding hydrochloric acid
- 3기타is removed by filtration
- 4기타The expected product precipitates
- 5여과After filtration
- 6기타drying
- 7기타it is purified as its hydrochloride
- 8기타before 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.