تفاعل #710509
ord-08be6ac03d714254b0303bbc09bd48d8
معادلة التفاعل
الكواشف
المذيبات
ظروف التفاعل
المعالجة
- 1ترشيحfiltering the resultant
- 2أخرىto remove palladium carbon
- 3أخرىdrying the resulting solution in vacuo
- 4workup.ADDITIONadding ethanol
- 5ترشيحfiltering the resultant
- 6أخرىto obtain a crude crystalline adenosine N1-oxide
- 7workup.DISSOLUTIONThe crude crystals were dissolved
- 8ترشيحfiltered
- 9درجة الحرارةice chilled for crystallization
- 10أخرىthe recrystallization step twice
الإجراء التجريبي
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%.