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

HRID 2112809
ノート
印刷プレビュー

反応式

HRID 2112809 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 is 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 is kept for 5 hours at this temperature. The reaction solution is cooled in the ice bath, and the precipitate formed is filtered and then washed with toluene until the product is virtually colorless. Subsequently it is dried at 50° C. in the circulating air dryer until the weight is constant. 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 min (method B).

後処理

  1. customthe precipitate formed
  2. filtrationis filtered
  3. washwashed with toluene until the product
  4. customSubsequently it is dried at 50° C. in the circulating air dryer until the weight
  5. custom4.7 min (method B)

出典と根拠

ORDレコード
ord-c5ddacf3307643809bb7889ce93f0956
出典データセット
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07524862B2

反応ノート

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