Triethylamine → 3-(Triethoxysilyl)propylacrylamide

HRID 54885ノート

反応式

HRID 54885 の反応式
[C:1](Cl)(=[O:4])[CH:2]=[CH2:3].N[CH2:7][CH2:8][CH2:9][Si:10]([O:17][CH2:18][CH3:19])([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13].C([N:22](CC)CC)C>ClCCl>[CH2:12]([O:11][Si:10]([O:17][CH2:18][CH3:19])([O:14][CH2:15][CH3:16])[CH2:9][CH2:8][CH2:7][C:2](=[CH2:3])[C:1]([NH2:22])=[O:4])[CH3:13]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 13140Acryloyl chlorideHCID 13521(3-Aminopropyl)triethoxysilane

生成物 1

HCID 187622113-(Triethoxysilyl)propylacrylamide収率 77%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of acryloyl chloride (8.5 mL, 105 mmol) in dry dichloromethane (250 mL) cooled to 0° C. was added dropwise a mixture of 3-aminopropyltriethoxysilane (23.5 mL, 100 mmol) and triethylamine (13.9 mL, 100 mmol) in dichloromethane (50 mL). After completion of addition the reaction mixture was stirred for 30 min, then filtered. The filtrate was concentrated to an oil, diluted with hexane (100 mL) and filtered. The resulting filtrate was concentrated to oil and distilled in vacuo. The product was obtained as a viscous liquid (21.2 g, 77%), b.p. 142-145/1 mm Hg.

後処理

  1. additionwas added dropwise
  2. additionAfter completion of addition the reaction mixture
  3. filtrationfiltered
  4. concentrationThe filtrate was concentrated to an oil
  5. additiondiluted with hexane (100 mL)
  6. filtrationfiltered
  7. concentrationThe resulting filtrate was concentrated to oil
  8. distillationdistilled in vacuo

出典と根拠

ORDレコード
ord-002083350cc34e8dbe3e7428d2f0b9f3
出典データセット
uspto-grants-1997_04
特許番号
US05624711

反応ノート

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