Ethylenediamine → 2,6-Diamino-N2-(2-aminoethyl)-5-nitropyridine

HRID 31847

반응식

HRID 31847 반응식
[NH2:1][C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[C:4](Cl)[N:3]=1.[NH2:12][CH2:13][CH2:14][NH2:15].[OH-].[Na+]>O>[NH2:12][CH2:13][CH2:14][NH:15][C:4]1[CH:5]=[CH:6][C:7]([N+:8]([O-:10])=[O:9])=[C:2]([NH2:1])[N:3]=1

참가 물질

5

반응물 3

HCID 3301EthylenediamineHCID 14798Sodium HydroxideHCID 27240356-Chloro-3-nitropyridin-2-ylamine

생성물 1

HCID 221423802,6-Diamino-N2-(2-aminoethyl)-5-nitropyridine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1 mmol of 2-amino-6-chloro-3-nitropyridine and 15 mmol of 1,2-diaminoethane were stirred at reflux for fourteen hours. The reaction mixture was concentrated in vacuo and solution of 1.5 mmol of NaOH in water was added. This solution was extracted twice with 95%/5% methylene chloride/methanol. The aqueous was then saturated with salt and extracted twice with 95%/5% acetonitrile/methanol and then finally extrated twice with 95%/5% ethylacetate/methanol. All organic fractions were combined and dried over sodium sulfate to obtain (2-aminoethyl)(6-amino-5-nitro(2-pyridyl))amine.

후처리

  1. temperatureat reflux for fourteen hours
  2. additionwas added
  3. extractionThis solution was extracted twice with 95%/5% methylene chloride/methanol
  4. extractionsaturated with salt and extracted twice with 95%/5% acetonitrile/methanol
  5. dry with materialdried over sodium sulfate

출처 및 근거

ORD 기록
ord-92d0d0ce25ff48e1be007eecd5189581
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07425557B2

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