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Water → 4-Cyclopropyl-3-fluoro-2-methoxybenzaldehyde

HRID 2272518
ノート
印刷プレビュー

反応式

HRID 2272518 の反応式
[CH3:1][O-:2].[Na+].[CH:4]1([C:7]2[CH:14]=[CH:13][C:10]([CH:11]=[O:12])=[C:9](F)[C:8]=2[F:16])[CH2:6][CH2:5]1.O>CO>[CH:4]1([C:7]2[CH:14]=[CH:13][C:10]([CH:11]=[O:12])=[C:9]([O:2][CH3:1])[C:8]=2[F:16])[CH2:6][CH2:5]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 3

HCID 962WaterHCID 10942334Sodium MethoxideHCID 904235484-Cyclopropyl-2,3-difluorobenzaldehyde

生成物 1

HCID 904232524-Cyclopropyl-3-fluoro-2-methoxybenzaldehyde収率 91.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

Sodium methoxide (28% methanol solution, 3.43 g) was added at room temperature to a methanol (100 mL) solution of 4-cyclopropyl-2,3-difluorobenzaldehyde (2.16 g), and the mixture was stirred at 70 C for 15 hours in a nitrogen atmosphere. Water was added to the reaction mixture, and methanol was distilled off under reduced pressure. The residue was subjected to 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. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate) to obtain the title compound (2.11 g)

後処理

  1. distillationwas distilled off under reduced pressure
  2. extractionThe residue was subjected to extraction with ethyl acetate
  3. washThe obtained organic layer was washed with water and saturated saline in this order
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)

出典と根拠

ORDレコード
ord-4aba2023b14a454095d2ad28d556132e
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09120777B2

反応ノート

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