反応 #710509

反応方程式

adenosine

hydrogen peroxide

hydrogen peroxide

→

adenosine N1-oxide

溶媒

ethanol

acetic acid

反応条件

後処理

1. 1
   ろ過filtering the resultant
2. 2
   その他to remove palladium carbon
3. 3
   その他drying the resulting solution in vacuo
4. 4
   workup.ADDITIONadding ethanol
5. 5
   ろ過filtering the resultant
6. 6
   その他to obtain a crude crystalline adenosine N1-oxide
7. 7
   workup.DISSOLUTIONThe crude crystals were dissolved
8. 8
   ろ過filtered
9. 9
   温度ice chilled for crystallization
10. 10
    その他the recrystallization step twice

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%.

出典