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2-Chlorobenzaldehyde → HCID 21276949、化合物

HRID 2292138
ノート
印刷プレビュー

反応式

HRID 2292138 の反応式
[C:1]([NH:5][C:6](=[O:11])/[CH:7]=[C:8](\[NH2:10])/[CH3:9])([CH3:4])([CH3:3])[CH3:2].[Cl:12][C:13]1[CH:20]=[CH:19][CH:18]=[CH:17][C:14]=1[CH:15]=O.[CH3:21][N:22]1[C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=2[N:24]=[C:23]1[CH2:31][CH2:32][CH2:33][O:34][CH2:35][C:36](=O)[CH2:37][C:38]([O:40][CH2:41][CH3:42])=[O:39]>C(O)C>[C:1]([NH:5][C:6]([C:7]1[CH:15]([C:14]2[CH:17]=[CH:18][CH:19]=[CH:20][C:13]=2[Cl:12])[C:37]([C:38]([O:40][CH2:41][CH3:42])=[O:39])=[C:36]([CH2:35][O:34][CH2:33][CH2:32][CH2:31][C:23]2[N:22]([CH3:21])[C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=3[N:24]=2)[NH:10][C:8]=1[CH3:9])=[O:11])([CH3:4])([CH3:2])[CH3:3]
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 69962-ChlorobenzaldehydeHCID 19864533HCID 19864533、化合物HCID 21276958HCID 21276958、化合物

生成物 1

HCID 21276949HCID 21276949、化合物収率 14.3%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

N-t-Butyl-3-aminocrotonamide (0.63 g), 2-chlorobenzaldehyde (0.56 g) and ethyl 4-[3-(1-methylbenzimidazol-2-yl)propoxy]-3-ketobutanoate (1.27 g) were dissolved in ethanol (16 ml) and stirred under reflux for 15 hours. The reaction mixture was cooled and the solvent removed under reduced pressure. The residue was chromatographed on silica eluting with 3% methanol in ethyl acetate. The fractions containing the product were combined and evaporated. Recrystallisation of the resulting foam from ethanol yielded the title compound as a white solid (0.33 g, 14%), m.p. 202° C. Found: C, 66.17; H, 6.92; N, 9.48. C32H39ClN4O4 requires C, 66.36; H, 6.79; N, 9.68%.

後処理

  1. temperatureunder reflux for 15 hours
  2. temperatureThe reaction mixture was cooled
  3. customthe solvent removed under reduced pressure
  4. customThe residue was chromatographed on silica eluting with 3% methanol in ethyl acetate
  5. additionThe fractions containing the product
  6. customevaporated
  7. customRecrystallisation of the resulting foam from ethanol

出典と根拠

ORDレコード
ord-c27ae321195640029b193d16ba75816b
出典データセット
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04801598

反応ノート

読み込み中…

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