Triethylamine → 3-(Triethoxysilyl)propylacrylamide

HRID 54885

반응식

HRID 54885 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 187622113-(Triethoxysilyl)propylacrylamide수율 77%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-002083350cc34e8dbe3e7428d2f0b9f3
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05624711

연결된 노트

불러오는 중…