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1,1-Dichloroacetone → 4,5-Difluoro-2-methoxybenzaldehyde

HRID 618706
ノート
印刷プレビュー

反応式

HRID 618706 の反応式
[F:1][C:2]1[CH:3]=[C:4]([O:9][CH3:10])[CH:5]=[CH:6][C:7]=1[F:8].C[C:12](C(Cl)Cl)=[O:13]>ClCCl.[Ti](Cl)(Cl)(Cl)Cl>[F:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([CH:12]=[O:13])=[C:4]([O:9][CH3:10])[CH:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 105671,1-DichloroacetoneHCID 5682503,4-Difluoroanisole

生成物 1

HCID 154345524,5-Difluoro-2-methoxybenzaldehyde収率 85.1%

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 6344Dichloromethane溶媒

実験手順

7.29 ml (66.3 mmol) of titanium tetrachloride were added while stirring to a solution, cooled to 0°, of 5.73 g (39.8 mmol) of 3,4-difluoroanisole in 30 ml of anhydrous dichloromethane. Subsequently, the mixture was treated dropwise over 10 minutes with 3.51 ml (39.6 mmol) of 1,1-dichloromethyl methyl ketone and stirred at room temperature for one hour. The mixture was poured into 100 ml of ice-water, extracted twice with 150 ml of dichloromethane each time and the combined organic phases were washed once with 100 ml of water and once with 100 ml of saturated sodium chloride solution. After drying over magnesium sulfate concentration was carried out in a vacuum. The crude product obtained was purified by column chromatography on silica gel (hexane/ethyl acetate 4:1). There were obtained 5.8 g (84%) of 4,5-difluoro-2-methoxybenzaldehyde as a white solid with m.p. 74°.

後処理

  1. stirringstirred at room temperature for one hour
  2. extractionextracted twice with 150 ml of dichloromethane each time
  3. washthe combined organic phases were washed once with 100 ml of water and once with 100 ml of saturated sodium chloride solution
  4. dry with materialAfter drying over magnesium sulfate concentration
  5. customThe crude product obtained
  6. customwas purified by column chromatography on silica gel (hexane/ethyl acetate 4:1)

出典と根拠

ORDレコード
ord-5e33f5ae1f524c438b65b7409c6f1890
出典データセット
uspto-grants-1999_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05955495

反応ノート

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