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

HRID 1074215ノート

反応式

HRID 1074215 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 9857164N-(3-(Triethoxysilyl)propyl)methacrylamide収率 38.4%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e3795e7e93fd4cda865327ab99985853
出典データセット
uspto-grants-1990_11
特許番号
US04973680

反応ノート

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