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Hydrochloric Acid → HCID 22445845、化合物

HRID 2375350
ノート
印刷プレビュー

反応式

HRID 2375350 の反応式
[C:1]1([CH2:7][CH2:8][NH:9][C:10](=[O:12])[CH3:11])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:13](Cl)(=[O:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[Cl-].[Cl-].[Cl-].[Al+3].Cl>[N+](C1C=CC=CC=1)([O-])=O>[C:13]([C:4]1[CH:5]=[CH:6][C:1]([CH2:7][CH2:8][NH:9][C:10](=[O:12])[CH3:11])=[CH:2][CH:3]=1)(=[O:20])[C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7412Benzoyl chlorideHCID 70143N-(2-phenylethyl)acetamideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 22445845HCID 22445845、化合物収率 34.3%

試薬・触媒・溶媒 1

HCID 7416Nitrobenzene溶媒2 回

反応条件

温度
50 °C

実験手順

N-(2-Phenylethyl)acetamide (49.01 mmol, 8.00 g) was introduced into nitrobenzene (40 ml). Benzoyl chloride (54.07 mmol, 7.60 g) was added thereto and then, at room temperature, aluminum tri-chloride (73.52 mmol, 9.80 g) was introduced in portions. The mixture was then heated at 50° C. for 8 h. The reaction mixture was poured into a mixture of ice and concentrated hydrochloric acid, and nitrobenzene was removed by steam distillation. The aqueous residue was extracted with ethyl acetate. The residue after concentration of the organic phase was chromatographed on silica gel (mobile phase dichloromethane/methanol (3% by volume)), resulting in 4.5 g of the title compound as orange oil.

後処理

  1. customwas removed by steam distillation
  2. extractionThe aqueous residue was extracted with ethyl acetate
  3. customThe residue after concentration of the organic phase was chromatographed on silica gel (mobile phase dichloromethane/methanol (3% by volume))

出典と根拠

ORDレコード
ord-cbb5fc12478c4562bac866e9c577c191
出典データセット
uspto-grants-2008_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07465744B2

反応ノート

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