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Hydrochloric Acid → 2-Methoxy-5-(1,1,2,2,2-pentafluoroethyl)benzaldehyde

HRID 2269260
ノート
印刷プレビュー

反応式

HRID 2269260 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:15])([F:14])[C:10]([F:13])([F:12])[F:11])=[CH:5][C:4]=1[CH:16]1OCCC[O:17]1.Cl>CC(C)=O>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:14])([F:15])[C:10]([F:11])([F:12])[F:13])=[CH:5][C:4]=1[CH:16]=[O:17]
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 313Hydrochloric AcidHCID 18677628HCID 18677628、化合物

生成物 1

HCID 186776122-Methoxy-5-(1,1,2,2,2-pentafluoroethyl)benzaldehyde収率 33.8%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a stirred solution of Compound 39 (1.0 g) in acetone (30 ml) was added conc. HCl (4 ml) at room temperature. The reaction mixture was stirred at room temperature for 5 h. The solvent was evaporated in vacuo and the residue was extracted with ether. The combined solution was washed with sat. NaHCO3 aq., and brine, dried(MgSO4) and concentrated in vacuo to give crude product (790 mg) as a yellow solid. The crude product was purified by column chromatography on silica gel with hexane-isopropyl ether(10:1-3:1) to give Compound 40 (275 mg) as a pale yellow solid.

後処理

  1. customThe solvent was evaporated in vacuo
  2. extractionthe residue was extracted with ether
  3. washThe combined solution was washed with sat. NaHCO3 aq., and brine, dried(MgSO4)
  4. concentrationconcentrated in vacuo
  5. customto give crude product (790 mg) as a yellow solid
  6. customThe crude product was purified by column chromatography on silica gel with hexane-isopropyl ether(10:1-3:1)

出典と根拠

ORDレコード
ord-759deea35bcc45adbf4024a3b051eb64
出典データセット
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06329396B1

反応ノート

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