Nitric Acid → 2,9-Dimethyl-5-nitro-1,10-phenanthroline

HRID 257614

反応式

HRID 257614 の反応式
[CH3:1][C:2]1[CH:15]=[CH:14][C:13]2[C:4](=[C:5]3[C:10](=[CH:11][CH:12]=2)[CH:9]=[CH:8][C:7]([CH3:16])=[N:6]3)[N:3]=1.[N+:17]([O-])([OH:19])=[O:18]>S(=O)(=O)(O)O>[N+:17]([C:11]1[CH:12]=[C:13]2[C:4]([N:3]=[C:2]([CH3:1])[CH:15]=[CH:14]2)=[C:5]2[C:10]=1[CH:9]=[CH:8][C:7]([CH3:16])=[N:6]2)([O-:19])=[O:18]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 652372,9-Dimethyl-1,10-phenanthroline

生成物 1

HCID 3797642,9-Dimethyl-5-nitro-1,10-phenanthroline

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

反応条件

温度
100 °C

実験手順

2,9-Dimethyl-1,10-phenanthroline (h) (20 g) was dissolved in a mixture of sulfuric acid (120 ml) and nitric acid (40 ml), and the mixture was heated at 100° C. for 12 hours with stirring. The resulting solution was poured into ice water (300 ml), and the formed precipitate was collected. The precipitate was dissolved in water (500 ml) and neutralized with sodium hydroxide. The resulting precipitate was collected and recrystallized from methanol (300 ml) to give the desired 5-nitro-2,9-dimethyl-1,10-phenanthroline (i) (yield=8.8 g).

後処理

  1. customthe formed precipitate was collected
  2. dissolutionThe precipitate was dissolved in water (500 ml)
  3. customThe resulting precipitate was collected
  4. customrecrystallized from methanol (300 ml)

出典と根拠

ORDレコード
ord-5decf9e2f16549c0a64c2625484c21b4
出典データセット
uspto-grants-1993_11
特許番号
US05262526

関連ノート

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