Sodium Hydroxide → 1,10-Phenanthrolin-5-amine

HRID 341910

反応式

HRID 341910 の反応式
[N+:1]([C:4]1[CH:17]=[C:16]2[C:11]([N:12]=[CH:13][CH:14]=[CH:15]2)=[C:10]2[C:5]=1[CH:6]=[CH:7][CH:8]=[N:9]2)([O-])=O.[OH-].[Na+]>C(O)(=O)C.Cl>[NH2:1][C:4]1[CH:17]=[C:16]2[C:11]([N:12]=[CH:13][CH:14]=[CH:15]2)=[C:10]2[C:5]=1[CH:6]=[CH:7][CH:8]=[N:9]2

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 727905-Nitro-1,10-phenanthroline

生成物 1

HCID 6069701,10-Phenanthrolin-5-amine収率 66.2%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒

反応条件

温度
100 °C

実験手順

In 3.0 ml of acetic acid was dissolved 1.37 g (5.8 mmol) of 5-nitro-1,10-phenanthroline. A solution prepared by dissolving 1.08 g (4.8 mmol) of stannic chloride (II) dihydrate in 2.2 ml of concentrated hydrochloric acid was added dropwise thereto, followed by stirring at 100° C. for 2 hours. The reaction mixture was made alkaline with a NaOH aqueous solution and extracted with chloroform. After chloroform was distilled off under reduced pressure, a yellow solid was obtained. This was recrystallized from tetrahydrofurane-hexane to obtain 0.75 g (66%) of the desired 5-amino-1,10-phenanthroline (Compound (2)).

後処理

  1. customA solution prepared
  2. additionwas added dropwise
  3. extractionextracted with chloroform
  4. distillationAfter chloroform was distilled off under reduced pressure
  5. customa yellow solid was obtained
  6. customThis was recrystallized from tetrahydrofurane-hexane

出典と根拠

ORDレコード
ord-af28943d36054b04a8bec810d584c985
出典データセット
uspto-grants-1999_01
特許番号
US05856479

関連ノート

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