반응 #3725

반응 방정식

1,3-Di-cyclopropylmethyl xanthine

nitric acid

→

product

수율 56.5%

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

수율 56.5%

용매

acetic acid

반응 조건

후처리

1. 1
   여과the resulting yellow precipitate filtered off
2. 2
   workup.DISSOLUTIONThe yellow crystals were dissolved in dichloromethane
3. 3
   세척washed with water
4. 4
   건조The separated organic layer was then dried over anhydrous sodium sulphate
5. 5
   농축concentrated in vacuo
6. 6
   기타The product crystallized from the
7. 7
   농축concentrate

실험 절차

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).

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