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

HRID 1288028

반응식

HRID 1288028 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 30318Osmium Tetroxide촉매HCID 962Water용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-958bac4161344cff9c486501b571a860
출처 데이터셋
uspto-grants-1976_10
특허 번호
US03987053

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