Water → 1-Azaphenanthrene-5,6-dione

HRID 1640029

反応式

HRID 1640029 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 199224561-Azaphenanthrene-5,6-dione収率 68%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
108 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-89ca7b4e2bf44a12a69fb07c6f292caa
出典データセット
uspto-grants-2012_02
特許番号
US08110685B2

関連ノート

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