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Hydrogen Peroxide → HCID 178507181、化合物

HRID 929321
ノート
印刷プレビュー

反応式

HRID 929321 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].C1N=C(N)C2N=CN([C@@H]3[O:34][C@H](CO)[C@@H](O)[C@@H]3O)C=2N=1.O.OO>C(O)(=O)C.[C].[Pd]>[C@@H:1]1([N:10]2[C:19]3[C:13](=[C:14]([N+:16]([O-:34])=[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 3

HCID 784Hydrogen Peroxide2 回HCID 323269H-Purin-6-amine, 9-beta-D-arabinofuranosyl-, hydrate (1:1)HCID 60961Adenosine

生成物 1

HCID 178507181HCID 178507181、化合物

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 176Acetic Acid
溶媒

実験手順

Twenty grams of adenosine with a product code of A9251-25G, commercialized by Sigma-Aldrich Japan K.K., Tokyo, Japan, was dispersed in one liter of acetic acid and admixed with 100 mL of 30% hydrogen peroxide solution, followed by stirring the resulting mixture at ambient temperature for five days. An excessive amount of the remaining hydrogen peroxide was decomposed by the addition of five grams of 5% palladium carbon, commercialized by Kawaken Fine Chemicals Co., Ltd., Tokyo, Japan, followed by filtering the mixture to remove the palladium carbon, drying the resulting solution in vacuo, adding ethanol to the dried product to disperse the formed crystals, and filtering the resulting mixture to obtain crude crystals of adenosine N1-oxide. Eight grams of adenosine N1-oxide with a purity of 99.5% was obtained by dissolving the crude crystals in ethanol by heating, filtering the resulting solution, ice-chilling the filtrate to effect recrystallization, and repeating these steps twice.

後処理

  1. filtrationby filtering the mixture
  2. customto remove the palladium carbon
  3. customdrying the resulting solution in vacuo
  4. additionadding ethanol to the dried product
  5. additionto disperse the formed crystals
  6. filtrationfiltering the resulting mixture

出典と根拠

ORDレコード
ord-2b32604384a4425db62ef4c56cd11770
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09295627B2

反応ノート

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