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Triethylamine → 4-Allyloxyphenyl methacrylate

HRID 1977003
ノート
印刷プレビュー

反応式

HRID 1977003 の反応式
[C:1]([O:6][C:7](=[O:11])[C:8]([CH3:10])=[CH2:9])(=O)[C:2]([CH3:4])=C.[CH2:12]([O:15][C:16]1C=CC(O)=[CH:18][CH:17]=1)[CH:13]=[CH2:14].C(N(CC)CC)C>CN(C)C1C=CN=CC=1.C1(C)C=CC=CC=1>[C:7]([O:6][C:1]1[CH:2]=[CH:4][C:12]([O:15][CH2:16][CH:17]=[CH2:18])=[CH:13][CH:14]=1)(=[O:11])[C:8]([CH3:10])=[CH2:9]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 8471TriethylamineHCID 12974Methacrylic anhydrideHCID 17138834-(Allyloxy)phenol

生成物 1

HCID 219971104-Allyloxyphenyl methacrylate収率 90%

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 1140Toluene溶媒

反応条件

温度
37 °C

実験手順

Methacrylic anhydride (6.92 g; 0.045 moles) was added dropwise to a chilled solution of purified 4-allyloxyphenol (7.0 g; 0.047 moles), triethylamine (3.55 g; 0.035 moles), 4-dimethylaminopyridine (0.43 g; 0.004 moles), 2-6-di-tert-butyl-4-methylphenol (0.018 g; 0.08 m moles) and toluene (20 ml) in a stirred 100 ml reaction flask fitted with a reflux condenser, magnetic stirrer and thermocouple probe. During the addition the reaction temperature increased to 37° C. The mixture was heated at 110° C. for 1.5 hour, cooled and washed sequentially with equal volumes of saturated sodium bicarbonate, dilute hydrochloric acid and water. The solution was dried over magnesium sulfate and the solvent removed under reduced pressure to yield 4-allyloxyphenyl methacrylate (8.3 g; 90% yield) as a clear yellow liquid. The structure of the monomer was confirmed by proton and infrared spectral analysis and GC analysis indicated a purity of 90%.

後処理

  1. customfitted with a reflux condenser, magnetic stirrer
  2. additionDuring the addition the reaction temperature
  3. temperatureThe mixture was heated at 110° C. for 1.5 hour
  4. temperaturecooled
  5. washwashed sequentially with equal volumes of saturated sodium bicarbonate, dilute hydrochloric acid and water
  6. dry with materialThe solution was dried over magnesium sulfate
  7. customthe solvent removed under reduced pressure

出典と根拠

ORDレコード
ord-56186130212a48998657fbb22b253177
出典データセット
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06231714B1

反応ノート

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