Diethyl Ether → 3-(2,4-Dichlorophenyl)-2-(4-chlorophenyl)propanal

HRID 1160688ノート

反応式

HRID 1160688 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][CH:10]([C:13]1[CH:18]=[CH:17][C:16]([Cl:19])=[CH:15][CH:14]=1)[CH2:11][OH:12].[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.CCOCC>C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[CH2:9][CH:10]([C:13]1[CH:14]=[CH:15][C:16]([Cl:19])=[CH:17][CH:18]=1)[CH:11]=[O:12]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 12391212HCID 12391212、化合物HCID 178418287HCID 178418287、化合物

生成物 1

HCID 222703593-(2,4-Dichlorophenyl)-2-(4-chlorophenyl)propanal

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 3-(2,4-dichlorophenyl)-2-(4-chorophenyl)propanol (Step B, 0.89 g, 2.8 mmol) in 20 mL CH2Cl2 was added crushed activated molecular sieves (4 g). After stirring at room temperature for 10 min, pyridinium chlorochromate (0.90 g, 4.2 mmol) was added. After stirring at room temperature for 1 h, CELITE diatomaceous earth (4 g) was added followed by 100 mL ether. The resulting mixture was filtered through a silica gel pad, which was washed with ether (2×50 mL). The filtrate was concentrated to dryness and azeotroped with toluene to give the title compound, which was used without further purification.

後処理

  1. customcrushed activated molecular sieves (4 g)
  2. stirringAfter stirring at room temperature for 1 h
  3. additionCELITE diatomaceous earth (4 g) was added
  4. filtrationThe resulting mixture was filtered through a silica gel pad, which
  5. washwas washed with ether (2×50 mL)
  6. concentrationThe filtrate was concentrated to dryness
  7. customazeotroped with toluene

出典と根拠

ORDレコード
ord-6e508a62da4440ea8cd09c981f29c57e
出典データセット
uspto-grants-2010_10
特許番号
US07816534B2

反応ノート

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