Ethanol, 2-amino-, 1-nitrate, nitrate (1:1) → N-cyano-N'-(2-nitroxyethyl)-2-pyridinecarboximidamide

HRID 374131

반응식

HRID 374131 반응식
[C:1]([N:3]=[C:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)OC)#[N:2].[N+]([O-])(O)=O.[O:17]([CH2:21][CH2:22][NH2:23])[N+:18]([O-:20])=[O:19].C[O-].[Na+]>CO>[C:1]([NH:3][C:4]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][N:8]=1)=[N:23][CH2:22][CH2:21][O:17][N+:18]([O-:20])=[O:19])#[N:2]

참가 물질

5

반응물 3

HCID 78397Ethanol, 2-amino-, 1-nitrate, nitrate (1:1)HCID 100121892-Pyridinecarboximidic acid, N-cyano-, methyl esterHCID 10942334Sodium Methoxide

생성물 1

HCID 10399160N-cyano-N'-(2-nitroxyethyl)-2-pyridinecarboximidamide수율 63%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl N-cyano-2-pyridinecarboximidate (0.50 g, 3.1 mmol) was dissolved in methanol (5 ml), 2-nitroxyethylamine nitrate (0.57 g, 3.4 mmol) was added, and sodium methoxide (0.18 g, 3.4 mmol) was further added gradually. The mixture was stirred at room temperature for 10 minutes. After the reaction was completed, the reaction solution was concentrated under reduced pressure, and the residue thus obtained was extracted with dichloromethane (50 ml×3). The dichloromethane layer was dried over anhydrous sodium sulfate and concentrated under reduced pressure. The concentrated residue was crystallized from dichloromethane-diethyl ether to give the title compound (0.44 g, 0.20 mmol, yield: 63%) as colorless needles.

후처리

  1. concentrationthe reaction solution was concentrated under reduced pressure
  2. customthe residue thus obtained
  3. extractionwas extracted with dichloromethane (50 ml×3)
  4. dry with materialThe dichloromethane layer was dried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe concentrated residue was crystallized from dichloromethane-diethyl ether

출처 및 근거

ORD 기록
ord-22f82108d5b148e989178e388a296ea0
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166347

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