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Hydrogen Peroxide → HCID 178507181, 화합물

HRID 623327
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HRID 623327 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 784Hydrogen Peroxide2회HCID 60961Adenosine

생성물 1

HCID 178507181HCID 178507181, 화합물

시약·촉매·용매 3

HCID 23938Palladium촉매HCID 176Acetic Acid용매HCID 702Ethanol용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-08be6ac03d714254b0303bbc09bd48d8
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09301968B2

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