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Aluminum(III) Chloride → HCID 10360821、化合物

HRID 1607673
ノート
印刷プレビュー

反応式

HRID 1607673 の反応式
[F:1][C:2]1[CH:20]=[C:19]([F:21])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][C:13]=1[N+:14]([O-:16])=[O:15])[C:8](Cl)=[O:9].[Cl-].[Al+3].[Cl-].[Cl-]>C1C=CC=CC=1>[F:1][C:2]1[CH:20]=[C:19]([F:21])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][C:13]=1[N+:14]([O-:16])=[O:15])[C:8]([C:2]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:3]=1)=[O:9]
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 6451240Aluminum(III) ChlorideHCID 10448313HCID 10448313、化合物

生成物 1

HCID 10360821HCID 10360821、化合物収率 184.6%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

A mixture of 3-(2,4-difluorophenoxy)-4-nitrobenzoic acid (2.1 g) and phosphorus pentachloride (1.6 g) in benzene (20 ml) was stirred for 2 hours at room temperature. The mixture was concentrated under reduced pressure to give crystals of 3-(2,4-difluorophenoxy)-4-nitrobenzoyl chloride (2.2 g). A solution of 3-(2,4-difluorophenoxy)-4-nitrobenzoyl chloride (2.2 g) in benzene (20 ml) was added to a mixture of aluminum chloride (2.4 g) in benzene (20 ml). The mixture was stirred overnight at ambient temperature and concentrated under reduced pressure. The residue was dissolved in chloroform, washed with diluted hydrochloric acid and water successively, dried over magnesium sulfate, and concentrated under reduced pressure. The residue was recrystallized from a mixture of hexane and ethanol to give crystals of 3-(2,4-difluorophenoxy)-4-nitrobenzophenone (2.3 g).

後処理

  1. concentrationconcentrated under reduced pressure
  2. dissolutionThe residue was dissolved in chloroform
  3. washwashed with diluted hydrochloric acid and water successively
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was recrystallized from a mixture of hexane and ethanol

出典と根拠

ORDレコード
ord-1cff1bf665124f5d8db33a18575e39aa
出典データセット
uspto-grants-1989_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04866091

反応ノート

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