2-Nitroanthraquinone → 2-Aminoanthraquinone

HRID 2071316

반응식

HRID 2071316 반응식
[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

참가 물질

4

반응물 1

HCID 39285932-Nitroanthraquinone

생성물 1

HCID 83412-Aminoanthraquinone수율 98.6%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fa34f681611840598a23d42a1b600a7d
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04046785

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