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

HRID 257614

반응식

HRID 257614 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

반응 조건

온도
100 °C

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-5decf9e2f16549c0a64c2625484c21b4
출처 데이터셋
uspto-grants-1993_11
특허 번호
US05262526

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