Nitric Acid → 1,3-Di-n-butyl-8-nitro Xanthine

HRID 3628

반응식

HRID 3628 반응식
[CH2:1]([N:5]1[C:14](=[O:15])[C:13]2[NH:12][CH:11]=[N:10][C:9]=2[N:8]([CH2:16][CH2:17][CH2:18][CH3:19])[C:6]1=[O:7])[CH2:2][CH2:3][CH3:4].[N+:20]([O-])([OH:22])=[O:21]>C(O)(=O)C>[CH2:1]([N:5]1[C:14](=[O:15])[C:13]2[NH:12][C:11]([N+:20]([O-:22])=[O:21])=[N:10][C:9]=2[N:8]([CH2:16][CH2:17][CH2:18][CH3:19])[C:6]1=[O:7])[CH2:2][CH2:3][CH3:4]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 1014211,3-Dibutylxanthine

생성물 1

HCID 99444751,3-Di-n-butyl-8-nitro Xanthine

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
5 °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.

후처리

  1. filtrationthe resulting yellow precipitate filtered off
  2. washwashed with water (50 ml)
  3. dissolutionThe yellow crystals were dissolved in dichloromethane
  4. washwashed twice with water
  5. dry with materialThe separated organic layer was then dried (anhydrous sodium sulphate)
  6. concentrationconcentrated
  7. customto give a crystalline product, yield 73 g (86%), m.pt 168° C.

출처 및 근거

ORD 기록
ord-cc12e5c031414063a4d8c42a97e5d896
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05734051

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