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

HRID 1075963

反応式

HRID 1075963 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1fb2a3c363db40bd84a88d7c913109b6
出典データセット
uspto-grants-1976_05
特許番号
US03954789

関連ノート

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