تفاعل #3725

معادلة التفاعل

1,3-Di-cyclopropylmethyl xanthine

nitric acid

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product

المردود 56.5%

1,3-Di-cyclopropylmethyl-8-nitro Xanthine

المردود 56.5%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe resulting yellow precipitate filtered off
2. 2
   workup.DISSOLUTIONThe yellow crystals were dissolved in dichloromethane
3. 3
   غسيلwashed with water
4. 4
   تجفيفThe separated organic layer was then dried over anhydrous sodium sulphate
5. 5
   تركيزconcentrated in vacuo
6. 6
   أخرىThe product crystallized from the
7. 7
   تركيزconcentrate

الإجراء التجريبي

1,3-Di-cyclopropylmethyl xanthine (20 g, 0,076 mol) was dissolved in acetic acid (33 ml) and then treated with concentrated nitric acid (13.2 g) at 87° C. After 1 hour, the mixture was cooled to 5° C. and the resulting yellow precipitate filtered off. The yellow crystals were dissolved in dichloromethane and washed with water. The separated organic layer was then dried over anhydrous sodium sulphate and concentrated in vacuo. The product crystallized from the concentrate to yield a yellow crystalline product yield 12.2 g, (56.5%), m.pt. 207° C. (with decomposition).

المصدر