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Bis(trimethylsilyl)chloromethane → Bis(trimethylsilyl)methylmethacrylate

HRID 480531
ノート
印刷プレビュー

反応式

HRID 480531 の反応式
[CH3:1][Si:2]([CH:5]([Si:7]([CH3:10])([CH3:9])[CH3:8])Cl)([CH3:4])[CH3:3].[C:11]([O-:16])(=[O:15])[C:12]([CH3:14])=[CH2:13].[Na+]>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].C1C2NC3C(=CC=CC=3)SC=2C=CC=1.C(#N)C>[CH3:1][Si:2]([CH:5]([O:16][C:11](=[O:15])[C:12]([CH3:14])=[CH2:13])[Si:7]([CH3:10])([CH3:9])[CH3:8])([CH3:4])[CH3:3]
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 2

HCID 552583Bis(trimethylsilyl)chloromethaneHCID 3255932Sodium methacrylate

生成物 1

HCID 18764812Bis(trimethylsilyl)methylmethacrylate収率 60%

試薬・触媒・溶媒 3

HCID 7108Phenothiazine触媒HCID 21218Trioctylmethylammonium chloride触媒
HCID 6342
Acetonitrile
溶媒

実験手順

Bis(trimethylsilyl)chloromethane (Aldrich) (14.68 g, 0.075 mole), sodium methacrylate (8.96 g, 0.0825 mole), Adogen 464 (Aldrich) (1.70 g), and phenothiazine (0.05 grams) were placed in a round bottom flask equipped with a condenser, mechanical stirrer and a nitrogen inlet. The flask was charged with 200 ml acetonitrile and heated to reflux while stirring. After 4 days, the mixture was filtered to remove the solids and the solvent was removed in a rotary evaporator. Fractional distillation under reduced pressure gave 10.90 grams (60% yield) of a clear liquid at 46-48° C. at 0.5 mm pressure.

後処理

  1. customequipped with a condenser, mechanical stirrer and a nitrogen inlet
  2. temperatureheated
  3. temperatureto reflux
  4. filtrationthe mixture was filtered
  5. customto remove the solids
  6. customthe solvent was removed in a rotary evaporator
  7. distillationFractional distillation under reduced pressure

出典と根拠

ORDレコード
ord-de947e5f70ac4014a4c75f782fec3f15
出典データセット
uspto-grants-2003_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06653048B2

反応ノート

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