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

HRID 3628

反応式

HRID 3628 の反応式
[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]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 1014211,3-Dibutylxanthine

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
5 °C

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-cc12e5c031414063a4d8c42a97e5d896
出典データセット
uspto-grants-1998_03
特許番号
US05734051

関連ノート

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