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

HRID 1288026

反応式

HRID 1288026 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>[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

5

反応物 3

HCID 702EthanolHCID 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-2deb680f90ff42e3ad9e05b5bf803237
出典データセット
uspto-grants-1976_10
特許番号
US03987053

関連ノート

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