Water → 1-Azaphenanthrene-5,6-dione

HRID 1640029

반응식

HRID 1640029 반응식
[N:1]1[C:14]2[CH:13]=[CH:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][CH:2]=1.[O:15]=I(OI(=O)=O)=O.[OH2:22]>C(O)(=O)C>[N:1]1[C:14]2[C:5](=[C:6]3[C:11](=[CH:12][CH:13]=2)[CH:10]=[CH:9][C:8](=[O:22])[C:7]3=[O:15])[CH:4]=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 6796Benzo(F)QuinolineHCID 159402Iodine pentoxide

생성물 1

HCID 199224561-Azaphenanthrene-5,6-dione수율 68%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
108 °C

실험 절차

A solution of 68.3 g (381 mmol) of 1-azaphenanthrene and 157 g (470 mmol) of iodopentoxide in acetic acid was stirred under heat at 108° C. for 2 hours. After the reaction liquid had been cooled to room temperature, water was added to the reaction liquid to crystallize the product, and then the crystals were filtered off. Subsequently, the resultant crystal was dissolved in chloroform, washed with an aqueous solution of sodium hydrogen carbonate and an aqueous solution of sodium thiosulfate, dried, and exsiccated by concentration, whereby 53.9 g of 1-azaphenanthrene-5,6-dione were obtained (68% yield).

후처리

  1. customAfter the reaction liquid
  2. temperaturehad been cooled to room temperature
  3. customto crystallize the product
  4. filtrationthe crystals were filtered off
  5. dissolutionSubsequently, the resultant crystal was dissolved in chloroform
  6. washwashed with an aqueous solution of sodium hydrogen carbonate
  7. dry with materialan aqueous solution of sodium thiosulfate, dried
  8. concentrationexsiccated by concentration

출처 및 근거

ORD 기록
ord-89ca7b4e2bf44a12a69fb07c6f292caa
출처 데이터셋
uspto-grants-2012_02
특허 번호
US08110685B2

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