Triethylamine → N-(3-(Triethoxysilyl)propyl)methacrylamide

HRID 1074215노트

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HRID 1074215 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][Si:5]([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8].C(N(CC)CC)C.[C:22](Cl)(=[O:26])[C:23]([CH3:25])=[CH2:24]>C1(C)C=CC=CC=1>[C:22]([NH:1][CH2:2][CH2:3][CH2:4][Si:5]([O:12][CH2:13][CH3:14])([O:6][CH2:7][CH3:8])[O:9][CH2:10][CH3:11])(=[O:26])[C:23]([CH3:25])=[CH2:24]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 13521(3-Aminopropyl)triethoxysilaneHCID 13528Methacryloyl chloride

생성물 1

HCID 9857164N-(3-(Triethoxysilyl)propyl)methacrylamide수율 38.4%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
0 °C

실험 절차

A solution of 3-aminopropyltriethoxysilane (20.0 g) in toluene (200 ml) was added to a 500 ml three neck flask equipped with magnetic stir bar, addition funnel, and nitrogen inlet. A total of 9.11 g of triethylamine was added to the solution and the solution was cooled to 0° C. in an ice bath. A total of 9.41 g of methacryloyl chloride was added dropwise to the reaction by the addition funnel at a rate such that the temperature did not exceed 5° C. The reaction was stirred overnight with gradual warming to room temperature. The reaction mixture was then washed 4 times with 200 ml of ice water, dried over magnesium sulfate and concentrated under vacuum. The yield was 38.4 percent and the reaction product was used without further purification.

후처리

  1. customequipped with magnetic stir bar, addition funnel, and nitrogen inlet
  2. customdid not exceed 5° C
  3. temperaturewith gradual warming to room temperature
  4. washThe reaction mixture was then washed 4 times with 200 ml of ice water
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under vacuum
  7. customThe yield was 38.4 percent and the reaction product was used without further purification

출처 및 근거

ORD 기록
ord-e3795e7e93fd4cda865327ab99985853
출처 데이터셋
uspto-grants-1990_11
특허 번호
US04973680

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