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

HRID 341910

반응식

HRID 341910 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 6069701,10-Phenanthrolin-5-amine수율 66.2%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 313Hydrochloric Acid용매

반응 조건

온도
100 °C

실험 절차

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)).

후처리

  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

출처 및 근거

ORD 기록
ord-af28943d36054b04a8bec810d584c985
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05856479

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