Triethylamine → N-cyano-N'-(2-nitroxyethyl)-2-furancarboximidamide

HRID 374188

반응식

HRID 374188 반응식
[C:1]([N:3]=[C:4]([C:7]1[O:8][CH:9]=[CH:10][CH:11]=1)OC)#[N:2].[N+]([O-])(O)=O.[O:16]([CH2:20][CH2:21][NH2:22])[N+:17]([O-:19])=[O:18].C(N(CC)CC)C>CO>[C:1]([NH:3][C:4]([C:7]1[O:8][CH:9]=[CH:10][CH:11]=1)=[N:22][CH2:21][CH2:20][O:16][N+:17]([O-:19])=[O:18])#[N:2]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 78397Ethanol, 2-amino-, 1-nitrate, nitrate (1:1)HCID 103969822-Furancarboximidic acid, N-cyano-, methyl ester

생성물 1

HCID 10105009N-cyano-N'-(2-nitroxyethyl)-2-furancarboximidamide수율 45%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Methyl N-cyano-2 furancarboximidate (0.32 g, 2.09 mmol) was dissolved in methanol (3 ml), 2-nitroxyethylamine nitrate (0.37 g, 2.19 mmol) and triethylamine (0.22 g, 2.19 mmol) were added. The mixture was stirred at room temperature for 16 hours. After the reaction was completed, the reaction solution was concentrated under reduced pressure, and the residue thus obtained was subjected to chromatography on a silica gel column (WAKO GEL C-200, 25 g) eluting with dichloromethane. The eluted fractions were concentrated under reduced pressure and crystallized from dichloromethane to give the title compound (0.20 g, 0.89 mmol, yield: 45%) as colorless crystals.

후처리

  1. concentrationthe reaction solution was concentrated under reduced pressure
  2. customthe residue thus obtained
  3. washeluting with dichloromethane
  4. concentrationThe eluted fractions were concentrated under reduced pressure
  5. customcrystallized from dichloromethane

출처 및 근거

ORD 기록
ord-51ea2438329247a5961018fa8602c387
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166347

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