Реакция #710509

Уравнение реакции

adenosine

hydrogen peroxide

hydrogen peroxide

→

adenosine N1-oxide

Растворители

ethanol

acetic acid

Условия реакции

Обработка

1. 1
   Фильтрацияfiltering the resultant
2. 2
   Другоеto remove palladium carbon
3. 3
   Другоеdrying the resulting solution in vacuo
4. 4
   workup.ADDITIONadding ethanol
5. 5
   Фильтрацияfiltering the resultant
6. 6
   Другоеto obtain a crude crystalline adenosine N1-oxide
7. 7
   workup.DISSOLUTIONThe crude crystals were dissolved
8. 8
   Фильтрацияfiltered
9. 9
   Температураice chilled for crystallization
10. 10
    Другоеthe recrystallization step twice

Методика

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%.

Источник