Sodium Acetate → 3-Acetoxypropyltrivinylsilane

HRID 217567

反応式

HRID 217567 の反応式
Cl[CH2:2][CH2:3][CH2:4][Si:5]([CH:10]=[CH2:11])([CH:8]=[CH2:9])[CH:6]=[CH2:7].[C:12]([O-:15])(=[O:14])[CH3:13].[Na+]>CN(C)C=O>[C:12]([O:15][CH2:2][CH2:3][CH2:4][Si:5]([CH:10]=[CH2:11])([CH:8]=[CH2:9])[CH:6]=[CH2:7])(=[O:14])[CH3:13]

参加物

4

反応物 2

HCID 517045Sodium AcetateHCID 23630656Trivinyl(3-chloropropyl)silane

生成物 1

HCID 579455963-Acetoxypropyltrivinylsilane収率 76%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

As shown in Reaction Scheme 24, 3-chloropropyltrivinylsilane (1.0 g, 5.35 mmol) and sodium acetate (0.87 g, 10.7 mmol) were dissolved in 17 mL of dimethylformamide (DMF), and the reaction mixture was heated at 120° C. for 12 hours. After the reaction, the organic layer was separated after addition of distilled water and ether. The organic layer was dried over MgSO4, concentrated by evaporation of solvent, and the resulting residue was purified by column chromatography (n-Hex: EA=10:1, Rf=0.4) to give 855 mg (76% yield) of pure 3-acetoxypropyltrivinylsilane.

後処理

  1. customAfter the reaction
  2. customthe organic layer was separated
  3. additionafter addition of distilled water and ether
  4. dry with materialThe organic layer was dried over MgSO4
  5. concentrationconcentrated by evaporation of solvent
  6. customthe resulting residue was purified by column chromatography (n-Hex: EA=10:1, Rf=0.4)

出典と根拠

ORDレコード
ord-672dfd5c3911452085a6ee1da2c6cf62
出典データセット
uspto-grants-2012_06
特許番号
US08197903B2

関連ノート

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