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Benzeneacetyl chloride, 4-bromo- → 2-(4-Bromophenyl)-1-phenylethan-1-one

HRID 2293966
ノート
印刷プレビュー

反応式

HRID 2293966 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].[Br:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][C:13](Cl)=[O:14])=[CH:8][CH:7]=1>C1C=CC=CC=1>[Br:5][C:6]1[CH:11]=[CH:10][C:9]([CH2:12][C:13]([C:6]2[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=2)=[O:14])=[CH:8][CH:7]=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 181552Benzeneacetyl chloride, 4-bromo-HCID 6451240Aluminum(III) Chloride

生成物 1

HCID 134590982-(4-Bromophenyl)-1-phenylethan-1-one

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

To a suspension of aluminum chloride (2.64 g, 19.8 mmol) in dry benzene (40 ml) was added a solution of 4-bromophenylacetyl chloride (4.63 g, 19.8 mmol) in 15 ml benzene over a period of 25 minutes under nitrogen. The resulting dark yellow solution was refluxed for six hours, and cooled to room temperature. Ice water (100 ml) was added, and the layers separated. The aqueous layer was extracted with benzene (1×50 ml). The combined organic portions were washed with water (2×60 ml), 10% NaOH (1×60 ml), water (1×60 ml), and brine (1×60 ml), and dried over magnesium sulfate. After filtration, concentration of the filtrate in vacuo afforded the ketone as 5.06 g of a white microcrystalline solid (93% yield). NMR indicated good purity. A portion was recrystallized from boiling petroleum ether/ethanol to give the ketone as colorless plates: m.p. 147.5°-149.0° C. (lit. m.p. 146°-147° C.; Huttel, R. et al., J. Chem. Ber. 93:1433 (1960)); 1H NMR δ8.02 (d, J=7.1 Hz, 2H), 7.63-7.46 (m, 5H), 7.16 (d, J=8.3, 2H), 4.27 (s, 2H).

後処理

  1. temperatureThe resulting dark yellow solution was refluxed for six hours
  2. customthe layers separated
  3. extractionThe aqueous layer was extracted with benzene (1×50 ml)
  4. washThe combined organic portions were washed with water (2×60 ml), 10% NaOH (1×60 ml), water (1×60 ml), and brine (1×60 ml)
  5. dry with materialdried over magnesium sulfate
  6. filtrationAfter filtration, concentration of the filtrate in vacuo

出典と根拠

ORDレコード
ord-468377f2f59a47688019dd73e5d466f9
出典データセット
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05688789

反応ノート

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