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Sodium Methoxide → 2,2',4'-Trifluoro-3-methoxybiphenyl-4-carbaldehyde

HRID 531067
ノート
印刷プレビュー

反応式

HRID 531067 の反応式
[CH3:1][O-:2].[Na+].[F:4][C:5]1[C:10](F)=[C:9]([CH:12]=[O:13])[CH:8]=[CH:7][C:6]=1[C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=1[F:21]>CO>[F:4][C:5]1[C:10]([O:2][CH3:1])=[C:9]([CH:12]=[O:13])[CH:8]=[CH:7][C:6]=1[C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=1[F:21]
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 10942334Sodium MethoxideHCID 1179922312,2',3,4'-Tetrafluoro-[1,1'-biphenyl]-4-carbaldehyde

生成物 1

HCID 1179920892,2',4'-Trifluoro-3-methoxybiphenyl-4-carbaldehyde収率 99.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Sodium methoxide (28% methanol solution, 5.64 g) was added at room temperature to a methanol (120 mL) solution of 2,2′,3,4′-tetrafluorobiphenyl-4-carbaldehyde (4.95 g), and the mixture was heated to reflux for 16 hours in a nitrogen atmosphere. The reaction mixture was cooled to room temperature, and then, the solvent was distilled off under reduced pressure. The obtained residue was diluted with ethyl acetate and water, followed by extraction with ethyl acetate. The obtained organic layer was washed with water and saturated saline in this order and dried over anhydrous magnesium sulfate, and then, the solvent was distilled off under reduced pressure to obtain the title compound (5.14 g).

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux for 16 hours in a nitrogen atmosphere
  3. distillationthe solvent was distilled off under reduced pressure
  4. additionThe obtained residue was diluted with ethyl acetate and water
  5. extractionfollowed by extraction with ethyl acetate
  6. washThe obtained organic layer was washed with water and saturated saline in this order
  7. dry with materialdried over anhydrous magnesium sulfate
  8. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-1a30248d054a40ff97bf48a168611ffe
出典データセット
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09353108B2

反応ノート

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