반응 #3724
ord-cc12e5c031414063a4d8c42a97e5d896
반응 방정식
1,3-Di-n-butylxanthine
nitric acid
→
1,3-Di-n-butyl-8-nitro Xanthine
반응 조건
온도
5°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1여과the resulting yellow precipitate filtered off
- 2세척washed with water (50 ml)
- 3workup.DISSOLUTIONThe yellow crystals were dissolved in dichloromethane
- 4세척washed twice with water
- 5건조The separated organic layer was then dried (anhydrous sodium sulphate)
- 6농축concentrated
- 7기타to give a crystalline product, yield 73 g (86%), m.pt 168° C.
실험 절차
1,3-Di-n-butylxanthine (73 g, 0.28 mol) was dissolved in acetic acid (120 ml) and then treated with concentrated nitric acid (49 g) at 87° C. After 1 hour, the mixture was cooled to 5° C., the resulting yellow precipitate filtered off and washed with water (50 ml). The yellow crystals were dissolved in dichloromethane and washed twice with water. The separated organic layer was then dried (anhydrous sodium sulphate) and concentrated to give a crystalline product, yield 73 g (86%), m.pt 168° C.