三乙胺 → 4-Allyloxyphenyl methacrylate

HRID 1977003

反应方程式

HRID 1977003 反应方程式
[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]

参与物

6

反应物 3

HCID 8471三乙胺HCID 12974甲基丙烯酸酐HCID 17138834-丙烯氧基苯酚

产物 1

HCID 219971104-Allyloxyphenyl methacrylate收率 90%

试剂、催化剂与溶剂 2

HCID 142844-二甲氨基吡啶(DMAP)催化剂HCID 1140甲苯溶剂

反应条件

温度
37 °C

实验过程

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%.

后处理

  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

来源与证据

ORD记录
ord-56186130212a48998657fbb22b253177
来源数据集
uspto-grants-2001_05
专利号
US06231714B1

关联笔记

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