HRID978966

反应详情

EQUATION

反应方程式

HRID 978966 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

5.05 g (0.05 mol) of dry triethylamine distilled in the presence of calcium hydride was added to 20 ml of anhydrous ether distilled in the presence of lithium aluminum hydride, and the mixture was cooled with ice in a nitrogen atmosphere. 0.86 g (0.01 mol) of methacrylic acid was added thereto and the mixture was stirred. While cooling the mixture with ice, 3.23 g (0.01 mol) of triphenylmethyl bromide dissolved in 10 ml of anhydrous ether was added thereto, whereby the reaction rapidly proceeded and triethylamine hydrobromide was precipitated. The reaction was continued for 2.5 hr until the salt was completely precipitated, and the resulting crystal was recovered by filtration. When the solvent and excess triethylamine were distilled off, triphenylmethyl methacrylate was obtained as a crystal, which was then recrystallized from ether to give 3.07 g (yield: 92.9%) of a colorless prismatic crystal.

WORKUP

后处理

  1. distillationdistilled in the presence of lithium aluminum hydride
  2. temperaturethe mixture was cooled with ice in a nitrogen atmosphere
  3. additionwas added
  4. customwhereby the reaction
  5. customtriethylamine hydrobromide was precipitated
  6. customwas completely precipitated
  7. filtrationthe resulting crystal was recovered by filtration
  8. distillationWhen the solvent and excess triethylamine were distilled off