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Sodium Carbonate → 2-amino-N'-hydroxypyridine-4-carboximidamide

HRID 1784548
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HRID 1784548 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][N:3]=1.Cl.[NH2:11][OH:12].C(=O)([O-])[O-].[Na+].[Na+]>O.C(O)C>[NH2:1][C:2]1[CH:7]=[C:6]([C:8]([NH:11][OH:12])=[NH:9])[CH:5]=[CH:4][N:3]=1
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참가 물질

6

반응물 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 70155242-Aminoisonicotinonitrile

생성물 1

HCID 1785133752-amino-N'-hydroxypyridine-4-carboximidamide수율 68.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

A stirred mixture of commercially available 2-amino-4-cyano-pyridine [CAS-No. 42182-27-4] (1.0 g, 8.39 mmol), hydroxylamine hydrochloride (1.17 g, 16.8 mmol) and sodium carbonate (0.89 g, 8.39 mol) in water (8 ml) and ethanol (16 ml) was heated under reflux conditions for 3 h. The reaction mixture was evaporated, water (10 ml) was added and the mixture stirred at room temperature for 1 h. The precipitate was collected by filtration to yield the title compound (0.87 g, 68%) as an off-white solid. MS (EI) 152.0 [(M)+]; mp 188° C.

후처리

  1. temperaturewas heated under reflux conditions for 3 h
  2. customThe reaction mixture was evaporated
  3. additionwater (10 ml) was added
  4. filtrationThe precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-23fc2512cf304762b3cda44243edf4a0
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07504404B2

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