Imidazole → 1-[4-(4-Chlorophenyl)butan-4-onyl]imidazole

HRID 442509ノート

反応式

HRID 442509 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.[CH:6]1[C:11]([C:12]([CH2:14][CH2:15][CH2:16]Cl)=[O:13])=[CH:10][CH:9]=[C:8]([Cl:18])[CH:7]=1>CN(C)C=O>[Cl:18][C:8]1[CH:7]=[CH:6][C:11]([C:12](=[O:13])[CH2:14][CH2:15][CH2:16][N:1]2[CH:5]=[CH:4][N:3]=[CH:2]2)=[CH:10][CH:9]=1

参加物

4

反応物 2

HCID 795ImidazoleHCID 27237814,4'-Dichlorobutyrophenone

生成物 1

HCID 190783351-[4-(4-Chlorophenyl)butan-4-onyl]imidazole

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a 0° C. slurry of 10.5 g. of imidazole in 15 ml. dry dimethylformamide was added 6.5 g. of γ,p-dichlorobutyrophenone and the mixture was stirred overnight at room temperature then one day at 60° C. The above solution was poured into 400 ml. of water and extracted three times with ethyl acetate. The combined extracts were washed with water, dried over magnesium sulfate and the solvent evaporated to afford 1-[4-(4-chlorophenyl)butan-4-onyl]imidazole, which was used in the next step. This material may be further purified, if necessary, through the nitrate salt.

後処理

  1. customTo a 0° C.
  2. customone day
  3. customat 60° C
  4. additionThe above solution was poured into 400 ml
  5. extractionof water and extracted three times with ethyl acetate
  6. washThe combined extracts were washed with water
  7. dry with materialdried over magnesium sulfate
  8. customthe solvent evaporated

出典と根拠

ORDレコード
ord-8638fe06652943ee8f370931966af829
出典データセット
uspto-grants-1977_08
特許番号
US04045568

反応ノート

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