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Hydrogen Peroxide → HCID 178507181、化合物

HRID 623327
ノート
印刷プレビュー

反応式

HRID 623327 の反応式
[C@@H:1]1([N:10]2[C:19]3[N:18]=[CH:17][N:16]=[C:14]([NH2:15])[C:13]=3[N:12]=[CH:11]2)[O:9][C@H:6]([CH2:7][OH:8])[C@@H:4]([OH:5])[C@H:2]1[OH:3].[OH:20]O>C(O)(=O)C.[Pd].C(O)C>[C@@H:1]1([N:10]2[C:19]3[C:13](=[C:14]([N+:16]([O-:20])=[CH:17][N:18]=3)[NH2:15])[N:12]=[CH:11]2)[O:9][C@H:6]([CH2:7][OH:8])[C@@H:4]([OH:5])[C@H:2]1[OH:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 784Hydrogen Peroxide2 回HCID 60961Adenosine

生成物 1

HCID 178507181HCID 178507181、化合物

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒

実験手順

Twenty grams of adenosine (commercialized by Sigma-Aldrich Corporation, St. Louis, Mo. USA, Product code: A9251-25G) was dispersed in one liter of acetic acid, admixed with 100 mL of hydrogen peroxide solution, and stirred at ambient temperature for five days. To the resulting solution was added five grams of 5% palladium on carbon, commercialized by Kawaken Fine Chemicals Co., Ltd, Tokyo, Japan, followed by decomposing an excessive amount of hydrogen peroxide, filtering the resultant to remove palladium carbon, drying the resulting solution in vacuo, adding ethanol to unstiffen the formed crystals, and filtering the resultant to obtain a crude crystalline adenosine N1-oxide. The crude crystals were dissolved by heating in two liters of ethanol, filtered, and ice chilled for crystallization, followed by repeating the recrystallization step twice to obtain eight grams of adenosine N1-oxide with a purity of 99.5%.

後処理

  1. filtrationfiltering the resultant
  2. customto remove palladium carbon
  3. customdrying the resulting solution in vacuo
  4. additionadding ethanol
  5. filtrationfiltering the resultant
  6. customto obtain a crude crystalline adenosine N1-oxide
  7. dissolutionThe crude crystals were dissolved
  8. filtrationfiltered
  9. temperatureice chilled for crystallization
  10. customthe recrystallization step twice

出典と根拠

ORDレコード
ord-08be6ac03d714254b0303bbc09bd48d8
出典データセット
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09301968B2

反応ノート

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