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4-Bromoaniline → N-(4-Bromophenyl)-3-oxobutanamide

HRID 734780
ノート
印刷プレビュー

反応式

HRID 734780 の反応式
[CH2:1]=[C:2]1[O:6][C:4](=[O:5])[CH2:3]1.[Br:7][C:8]1[CH:14]=[CH:13][C:11]([NH2:12])=[CH:10][CH:9]=1>C1(C)C=CC=CC=1>[Br:7][C:8]1[CH:14]=[CH:13][C:11]([NH:12][C:4](=[O:5])[CH2:3][C:2](=[O:6])[CH3:1])=[CH:10][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 78074-BromoanilineHCID 12661Diketene

生成物 1

HCID 598820N-(4-Bromophenyl)-3-oxobutanamide

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

A solution of 25.72 mL (336 mmol) of diketene in 100 mL of toluene was added dropwise at 90° C. to a solution of 51.0 g (288 mmol) of 4-bromoaniline in 200 mL of toluene and the reaction mixture was kept at this temperature for 5 hours. The reaction solution was cooled in the ice bath, and the precipitate formed was filtered and washed with toluene until the product was virtually colorless. Subsequently it was dried at 50° C. in the circulating air dryer until a constant weight was obtained. Yield: 50.0 g (68% of theoretical); C10H10BrNO2 (M=256.096); calc.: molpeak (M+H)+: 256/258 (Br); found: molpeak (M+H)+: 256/258 (Br); HPLC-MS: 4.7 minutes (method B).

後処理

  1. customthe precipitate formed
  2. filtrationwas filtered
  3. washwashed with toluene until the product
  4. customSubsequently it was dried at 50° C. in the circulating air dryer until a constant weight
  5. customwas obtained
  6. custom4.7 minutes (method B)

出典と根拠

ORDレコード
ord-6c3b42c3741f4d3b8268e01f62edd893
出典データセット
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07592358B2

反応ノート

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