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Methylamine → 4-Methylamino-3-nitroquinoline

HRID 1789414
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HRID 1789414 반응식
[CH3:1][NH2:2].Cl[C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]=[CH:6][C:5]=1[N+:14]([O-:16])=[O:15]>O>[CH3:1][NH:2][C:4]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[N:7]=[CH:6][C:5]=1[N+:14]([O-:16])=[O:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 112758084-Chloro-3-nitroquinoline

생성물 1

HCID 139583214-Methylamino-3-nitroquinoline

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a stirred solution of 40% aqueous methylamine was added, in small portions, 30.Og (0.144 mole) of 4-chloro-3-nitroquinoline. The reaction mixture was heated at its reflux temperature for about 0.75 hour. After cooling, the mixture was poured into 300 ml of water. The solid was separated by filtration, and was then suspended in 300 ml of water. Acidification with 6N hydrochloric acid to pH 3 to 4 effected dissolution of most of the solid. Filtration was followed by basification of the filtrate with concentrated ammonium hydroxide to pH 8 to 10 to provide a yellow precipitate. The solid was separated by filtration, washed with water, and recrystallized from ethanol to provide yellow 4-methylamino-3-nitroquinoline, m.p. 168-170° C. Analysis: Calculated for C10H9N3O2 %C, 59.1; %H, 4.5: %N, 20.7: Found: %C, 59.0; %H, 4.2; %N, 20.8.

후처리

  1. temperatureThe reaction mixture was heated at its
  2. temperaturereflux temperature for about 0.75 hour
  3. temperatureAfter cooling
  4. customThe solid was separated by filtration
  5. dissolutiondissolution of most of the solid
  6. filtrationFiltration
  7. customto provide a yellow precipitate
  8. customThe solid was separated by filtration
  9. washwashed with water
  10. customrecrystallized from ethanol

출처 및 근거

ORD 기록
ord-701fcea6be6145faa217161bfc2ee4fd
출처 데이터셋
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04689338

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