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Imidazole → 2-Fluoro-5-methoxy-3-(2-triisopropylsilanyloxyethoxymethyl)benzaldehyde

HRID 1161581
ノート
印刷プレビュー

反応式

HRID 1161581 の反応式
[F:1][C:2]1[C:9]([CH2:10][O:11][CH2:12][CH2:13][OH:14])=[CH:8][C:7]([O:15][CH3:16])=[CH:6][C:3]=1[CH:4]=[O:5].N1C=CN=C1.Cl[Si:23]([CH:30]([CH3:32])[CH3:31])([CH:27]([CH3:29])[CH3:28])[CH:24]([CH3:26])[CH3:25].O>CN(C=O)C>[F:1][C:2]1[C:9]([CH2:10][O:11][CH2:12][CH2:13][O:14][Si:23]([CH:30]([CH3:32])[CH3:31])([CH:27]([CH3:29])[CH3:28])[CH:24]([CH3:26])[CH3:25])=[CH:8][C:7]([O:15][CH3:16])=[CH:6][C:3]=1[CH:4]=[O:5]
参加物反応条件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 795ImidazoleHCID 962WaterHCID 139400Triisopropylsilyl chlorideHCID 595168732-Fluoro-3-(2-hydroxyethoxymethyl)-5-methoxybenzaldehyde

生成物 1

HCID 595172852-Fluoro-5-methoxy-3-(2-triisopropylsilanyloxyethoxymethyl)benzaldehyde収率 103.7%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
50 °C

実験手順

2-Fluoro-3-(2-hydroxyethoxymethyl)-5-methoxybenzaldehyde (305 mg) was dissolved in 3 ml of DMF, and 300 mg of imidazole and 283 mg of chlorotriisopropylsilane were added thereto. The resulting mixture was stirred at 50° C. for 2 hours, and then water was added thereto. The mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate. The desiccating agent was removed by filtration, and the filtrate was concentrated under reduced pressure to give a crude product of the title compound (533 mg).

後処理

  1. extractionThe mixture was extracted with ethyl acetate
  2. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
  3. customThe desiccating agent was removed by filtration
  4. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-59dfd01664a446e8b6cb5dfd144219f5
出典データセット
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07816522B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート