Ethanol, 2-amino-, 1-nitrate, nitrate (1:1) → N-cyano-N'-(2-nitroxyethyl)-4-pyridinecarboximidamide

HRID 374172

반응식

HRID 374172 반응식
[C:1]([N:3]=[C:4]([C:9]1[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=1)OC(C)C)#[N:2].[N+]([O-])(O)=O.[O:19]([CH2:23][CH2:24][NH2:25])[N+:20]([O-:22])=[O:21].C[O-].[Na+]>CO>[C:1]([NH:3][C:4]([C:9]1[CH:10]=[CH:11][N:12]=[CH:13][CH:14]=1)=[N:25][CH2:24][CH2:23][O:19][N+:20]([O-:22])=[O:21])#[N:2]

참가 물질

5

반응물 3

HCID 78397Ethanol, 2-amino-, 1-nitrate, nitrate (1:1)HCID 10012715Isopropyl N-cyano-4-pyridinecarboximidateHCID 10942334Sodium Methoxide

생성물 1

HCID 10059957N-cyano-N'-(2-nitroxyethyl)-4-pyridinecarboximidamide수율 61.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Isopropyl N-cyano-4-pyridinecarboximidate (0.50 g, 2.6 mmol) was dissolved in methanol (10 ml), and 2-nitroxyethylamine nitrate (0.57 g, 2.9 mmol) and sodium methoxide (0.18 g, 2.9 mmol) were added. The mixture was stirred at room temperature for 10 minutes. After the reaction was completed, the reaction solution was concentrated under reduced pressure. 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 residual concentrate was crystallized from dichloromethane-diethyl ether to give the title compound (0.37 g, 1.6 mmol, yield: 61%) 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. concentrationThe residual concentrate
  7. customwas crystallized from dichloromethane-diethyl ether

출처 및 근거

ORD 기록
ord-d01f77a329184a65851e0541cd12a4d8
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166347

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