1,2-Dimethoxyethane → 1-Methyl-2-nitro-1H-imidazole-5-carboxaldehyde

HRID 1288028

反応式

HRID 1288028 の反応式
[CH3:1][N:2]1[C:6]([CH:7]=C)=[CH:5][N:4]=[C:3]1[N+:9]([O-:11])=[O:10].C[O:13]CCOC>O=[Os](=O)(=O)=O.O>[CH3:1][N:2]1[C:6]([CH:7]=[O:13])=[CH:5][N:4]=[C:3]1[N+:9]([O-:11])=[O:10]

参加物

5

反応物 2

HCID 80711,2-DimethoxyethaneHCID 932151-ME-2-NO2-5-Vinyl imidazole

生成物 1

HCID 1003901-Methyl-2-nitro-1H-imidazole-5-carboxaldehyde収率 63%

試薬・触媒・溶媒 2

HCID 30318Osmium Tetroxide触媒HCID 962Water溶媒

実験手順

To a solution of 0.67 g. of 1-methyl-2-nitro-5-vinylimidazole in 20 ml. of 1,2-dimethoxyethane, a solution of 2 g. of NaIO4 in 5 ml. of water, followed by 0.025 g. of OsO4 is added with stirring at room temperature. After stirring for four hours, the mixture is allowed to stand overnight. The residue which is obtained by evaporation of the reaction medium to dryness under vacuum is extracted with ethyl acetate. The resulting solution after filtering is concentrated, yielding 0.43 g. of a product which, after crystallization from ethyl acetate, melts at 114°-115° C. Yield 63%.

後処理

  1. stirringAfter stirring for four hours
  2. customThe residue which is obtained by evaporation of the reaction medium to dryness under vacuum
  3. extractionis extracted with ethyl acetate
  4. filtrationThe resulting solution after filtering
  5. concentrationis concentrated
  6. customyielding 0.43 g
  7. customof a product which, after crystallization from ethyl acetate, melts at 114°-115° C

出典と根拠

ORDレコード
ord-958bac4161344cff9c486501b571a860
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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