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Dimethylformamide → HCID 13861691、化合物

HRID 1066629
ノート
印刷プレビュー

反応式

HRID 1066629 の反応式
C([Si](C)(C)[O:6][C:7]1[C:8]([F:23])=[C:9]([CH:12]=[C:13](O[Si](C(C)(C)C)(C)C)[CH:14]=1)[CH:10]=[O:11])(C)(C)C.[F-].[K+].[CH3:28]I.CN([CH:33]=[O:34])C>O>[F:23][C:8]1[C:7]([O:6][CH3:28])=[CH:14][C:13]([O:34][CH3:33])=[CH:12][C:9]=1[CH:10]=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 522689Potassium FluorideHCID 138616903,5-Bis{[tert-butyl(dimethyl)silyl]oxy}-2-fluorobenzaldehyde

生成物 1

HCID 13861691HCID 13861691、化合物収率 60%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of the 3,5-bis-(tert-butyl-dimethyl-silanyloxy)-2-fluoro-benzaldehyde (3.0 g, 7.8 mmol) obtained in Example 251.1, potassium fluoride (1.81 g, 31.2 mmol), methyl iodide (1.17 ml, 18.7 mmol) and DMF (25 ml) was stirred for 2 h. at room temperature. Water (25 ml) was added and the mixture was extracted with diethyl ether. The organic phase was washed with water, dried, filtered and concentrated. The residue was purified by chromato-graphy (SiO2, cyclohexane/EtOAc 18:1=>1:1). There was obtained 0.87 g (60%) of 2-fluoro-3,5-dimethoxy-benzaldehyde as a colorless solid.

後処理

  1. extractionthe mixture was extracted with diethyl ether
  2. washThe organic phase was washed with water
  3. customdried
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified by chromato-graphy (SiO2, cyclohexane/EtOAc 18:1=>1:1)

出典と根拠

ORDレコード
ord-5f623bc892e447cd8aaa52b49a14453c
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06242644B1

反応ノート

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