Ethanol → 1-(1-Methyl-2-nitro-1H-imidazol-5-yl)ethane-1,2-diol

HRID 1075963

반응식

HRID 1075963 반응식
[CH3:1][N:2]1[C:6](C=C)=[CH:5][N:4]=[C:3]1[N+:9]([O-:11])=[O:10].[CH2:12]([OH:14])[CH3:13].[O-:15][Mn](=O)(=O)=O.[K+].[O-]S([O-])(=O)=O.[Mg+2]>O>[CH3:1][N:2]1[C:6]([CH:13]([OH:15])[CH2:12][OH:14])=[CH:5][N:4]=[C:3]1[N+:9]([O-:11])=[O:10]

참가 물질

6

반응물 4

HCID 702EthanolHCID 24083Sulfuric acid magnesium salt (1:1)HCID 932151-ME-2-NO2-5-Vinyl imidazoleHCID 516875Potassium Permanganate

생성물 1

HCID 232737231-(1-Methyl-2-nitro-1H-imidazol-5-yl)ethane-1,2-diol

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a solution of 6.2 g. of 1-methyl-2-nitro-5-vinylimidazole in 570 ml. of ethanol cooled to about -10° C., a solution of 5.46 g. of KMnO4 and 8.85 g. of MgSO4 .7H2O in 750 ml. of H2O is added with stirring. The reaction mixture is filtered through Celite and washed with ethanol. The filtrate is concentrated to dryness under vacuum at 50° C., and the residue is taken up with acetone. The resulting solution is filtered and concentrated to dryness under vacuum. The resulting solid is crystallized from methyl ethyl ketone. Yield 3.15 g. (41.6%), m.p. 119°-121° C.

후처리

  1. filtrationThe reaction mixture is filtered through Celite
  2. washwashed with ethanol
  3. concentrationThe filtrate is concentrated to dryness under vacuum at 50° C.
  4. filtrationThe resulting solution is filtered
  5. concentrationconcentrated to dryness under vacuum
  6. customThe resulting solid is crystallized from methyl ethyl ketone

출처 및 근거

ORD 기록
ord-1fb2a3c363db40bd84a88d7c913109b6
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03954789

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