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Water → 3-[3-[2-(4-Bromophenyl)-5,5-dimethyl-1,3-dioxane-2-yl]propoxy]benzonitrile

HRID 747711
ノート
印刷プレビュー

反応式

HRID 747711 の反応式
[H-].[Na+].[OH:3][C:4]1[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=1)[C:7]#[N:8].[Br:12][C:13]1[CH:18]=[CH:17][C:16]([C:19]2([CH2:27][CH2:28][CH2:29]Cl)[O:24][CH2:23][C:22]([CH3:26])([CH3:25])[CH2:21][O:20]2)=[CH:15][CH:14]=1.O>CN(C)C=O>[Br:12][C:13]1[CH:14]=[CH:15][C:16]([C:19]2([CH2:27][CH2:28][CH2:29][O:3][C:4]3[CH:5]=[C:6]([CH:9]=[CH:10][CH:11]=3)[C:7]#[N:8])[O:20][CH2:21][C:22]([CH3:25])([CH3:26])[CH2:23][O:24]2)=[CH:17][CH:18]=1
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 962WaterHCID 133943-CyanophenolHCID 24758Sodium hydrideHCID 126147752-(4-Bromophenyl)-2-(3-chloropropyl)-5,5-dimethyl-1,3-dioxane

生成物 1

HCID 688339843-[3-[2-(4-Bromophenyl)-5,5-dimethyl-1,3-dioxane-2-yl]propoxy]benzonitrile

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒
2 回

実験手順

236 mg (5.9 mmol) of sodium hydride (oily, 60%) was stirred in dimethylformamide. 691 mg (5.8 mmol) of 3-hydroxybenzonitrile was added thereto under cooling with ice. After stirring at room temperature for 30 minutes, a solution of 2 g (5.75 mmol) of 2-(4-bromophenyl)-2-(3-chloropropyl)-5,5-dimethyl-1,3-dioxane in dimethylformamide was added to the reaction mixture, and they were stirred at 100° C. overnight. Water was added to the mixture. After the extraction with ethyl acetate, the organic layer was washed with 1 N aqueous sodium hydroxide solution and saturated aqueous common salt solution and dried over anhydrous magnesium sulfate. The solvent was evaporated to obtain the crude title compound.

後処理

  1. temperatureunder cooling with ice
  2. stirringwere stirred at 100° C. overnight
  3. extractionAfter the extraction with ethyl acetate
  4. washthe organic layer was washed with 1 N aqueous sodium hydroxide solution and saturated aqueous common salt solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated

出典と根拠

ORDレコード
ord-c89b107a172a4c6680b496a1efeacb7b
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07396844B1

反応ノート

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