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Methylamine → 4-Methylamino-3-nitroquinoline

HRID 255516
ノート
印刷プレビュー

反応式

HRID 255516 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6329MethylamineHCID 112758084-Chloro-3-nitroquinoline

生成物 1

HCID 139583214-Methylamino-3-nitroquinoline

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred solution of 40% aqueous methylamine was added, in small portions, 30.0 g (0.144 mole) of 4-chloro-3-nitroquinoline. The reaction mixture was then heated at its reflux temperature for about 0.75 hour. After cooling, the mixture was poured in 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.

後処理

  1. temperatureThe reaction mixture was then 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

出典と根拠

ORDレコード
ord-d794f459c09e484fa961ea9d92ad8a4c
出典データセット
uspto-grants-1987_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04698348

反応ノート

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