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2-Nitroanthraquinone → 2-Aminoanthraquinone

HRID 2071316
ノート
印刷プレビュー

反応式

HRID 2071316 の反応式
[N+:1]([C:4]1[CH:17]=[CH:16][C:15]2[C:14](=[O:18])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:19])[C:6]=2[CH:5]=1)([O-])=O>[C].[Pd].O>[NH2:1][C:4]1[CH:17]=[CH:16][C:15]2[C:14](=[O:18])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:19])[C:6]=2[CH:5]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 39285932-Nitroanthraquinone

生成物 1

HCID 83412-Aminoanthraquinone収率 98.6%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

2.5 g (0.01 mole) of 2-nitroanthraquinone (purity above 99%) containing about 10% of particles having a particle diameter of more than 100 microns was placed in a 200 ml. electromagnetically stirred autoclave together with 25 g of small glass balls each with a diameter of 1 mm, 75 g of water and 0.025 g of 5% palladium-carbon. The inside of the autoclave was purged with hydrogen, and then, the 2-nitroanthraquinone was hydrogenated with stirring at a temperature of 100° C. and a pressure of 2 to 6 Kg/cm2.G. The reaction proceeded smoothly, and stopped in 4 hours with the absorption of a theoretical amount of hydrogen. The reaction mixture was filtered, and the 22 g of conc. sulfuric acid was added to the filtrate mass to dissolve the reaction product. Then, the catalyst and the small glass balls were separated by filtration. The filtrate was diluted with water. The precipitated crystals were collected by filtration to afford 2.2 g of 2-aminoanthraquinone. The purity of the product was 99%, and its yield was almost quantitative.

後処理

  1. customThe inside of the autoclave was purged with hydrogen
  2. customstopped in 4 hours with the absorption of a theoretical amount of hydrogen
  3. filtrationThe reaction mixture was filtered
  4. additionthe 22 g of conc. sulfuric acid was added to the filtrate mass
  5. dissolutionto dissolve the reaction product
  6. customThen, the catalyst and the small glass balls were separated by filtration
  7. additionThe filtrate was diluted with water
  8. filtrationThe precipitated crystals were collected by filtration

出典と根拠

ORDレコード
ord-fa34f681611840598a23d42a1b600a7d
出典データセット
uspto-grants-1977_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04046785

反応ノート

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