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Pyridine → HCID 19875859、化合物

HRID 1086206
ノート
印刷プレビュー

反応式

HRID 1086206 の反応式
[CH3:1][CH:2]([CH3:19])[CH:3]([C:9]1[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([N+:16]([O-:18])=[O:17])[CH:10]=1)[N:4]1[CH:8]=[N:7][CH:6]=[N:5]1.N1C=CC=CC=1.[Cl:26][C:27]1[CH:32]=[CH:31][C:30]([CH2:33][C:34](Cl)=[O:35])=[CH:29][CH:28]=1>ClCCl>[Cl:26][C:27]1[CH:32]=[CH:31][C:30]([CH2:33][C:34]([NH:15][C:12]2[CH:13]=[CH:14][C:9]([CH:3]([N:4]3[CH:8]=[N:7][CH:6]=[N:5]3)[CH:2]([CH3:19])[CH3:1])=[CH:10][C:11]=2[N+:16]([O-:18])=[O:17])=[O:35])=[CH:29][CH:28]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 906924-Chlorophenylacetyl chlorideHCID 19875831HCID 19875831、化合物

生成物 1

HCID 19875859HCID 19875859、化合物収率 69.9%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirred and cooled (5° C.) solution of 10 parts of 4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]-2-nitrobenzenamine and 6.7 parts of pyridine in 195 parts of dichloromethane was added a solution of 14.4 parts of 4-chlorobenzeneacetyl chloride in 39 parts of dichloromethane under nitrogen atmosphere. After stirring overnight at room temperature, the reaction mixture was washed with water, dried, filtered and evaporated. The residue was purified by column chromatography over silica gel using a mixture of dichloromethane and methanol (99:1 by volume) as eluent. The eluent of the desired fraction was evaporated, yielding 11 parts (69.9%) of 4-chloro-N-[4-[2-methyl-1-(1H-1,2,4-triazol-1-yl)propyl]-2-nitrophenyl]benzeneacetamide (interm. 112).

後処理

  1. stirringAfter stirring overnight at room temperature
  2. washthe reaction mixture was washed with water
  3. customdried
  4. filtrationfiltered
  5. customevaporated
  6. customThe residue was purified by column chromatography over silica gel using
  7. additiona mixture of dichloromethane and methanol (99:1 by volume) as eluent
  8. customThe eluent of the desired fraction was evaporated

出典と根拠

ORDレコード
ord-6eba9c8427ba4e2e976a30de79086ba2
出典データセット
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05028606

反応ノート

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