Carbon Dioxide → 1-Aminoanthraquinone

HRID 1065028

반응식

HRID 1065028 반응식
[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[CH:5]=[CH:4][C:3]=1C(O)=O.[OH-].[NH4+].C(=O)=O>[Zn].O>[NH2:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[C:7](=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 280Carbon DioxideHCID 67012-Anthracenecarboxylic acid, 1-amino-9,10-dihydro-9,10-dioxo-HCID 14923Ammonium Hydroxide

생성물 1

HCID 67101-Aminoanthraquinone수율 83.3%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 962Water용매

실험 절차

To a three-necked round-bottomed flask equipped with stirrer and reflux condenser was added 2 g (0.007 mole) 1-aminoanthraquinone-2-carboxylic acid, 0.5 g (0.0018) zinc dust, 5 ml of 30% ammonium hydroxide solution and 30 ml of water. The resulting mixture was refluxed gently until evolution of carbon dioxide ceased, ca. 30 minutes. The mixture was then filtered while hot, and the filter cake was washed with water. The wet cake containing the zinc catalyst was heated over a steam bath with 50% sulfuric acid for one hour. Water was added and the solid product was collected by filtration and washed with water until acid-free. The product was dried to give 1.3 g (83.3% yield) of more than 90% pure 1-aminoanthraquinone.

후처리

  1. customTo a three-necked round-bottomed flask equipped with stirrer
  2. temperaturereflux condenser
  3. filtrationThe mixture was then filtered while hot, and the filter cake
  4. washwas washed with water
  5. additionThe wet cake containing the zinc catalyst
  6. temperaturewas heated over a steam bath with 50% sulfuric acid for one hour
  7. additionWater was added
  8. filtrationthe solid product was collected by filtration
  9. washwashed with water until acid-free
  10. customThe product was dried

출처 및 근거

ORD 기록
ord-679e3688a90d4ce6925eb4f37512933f
출처 데이터셋
uspto-grants-1982_05
특허 번호
US04328160

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