反应详情

A solution of 86 g. (1 mole) of methacrylic acid in 120 ml. benzene was reacted with 67.2 g. (1.2 moles) of propargyl alcohol in the presence of 4 g. of p-toluenesulfonic acid as a catalyst and 0.4 g. p-tertbutylcatechol as an inhibitor. The reaction mixture was stirred and heated to reflux under nitrogen until 18 g. of water was azeotroped over into a Dean-Stark trap. The reaction mixture was neutralized with saturated sodium carbonate aqueous solution, washed with deionized water three times and dried over sodium carbonate. The solvent was removed on a Rotavapor. Vacuum distillation of the residue in the presence of the inhibitor gave a 75% yield of propargyl methacrylate obtained as a clear colorless liquid.

1. temperatureheated
2. temperatureto reflux under nitrogen until 18 g
3. customof water was azeotroped over into a Dean-Stark trap
4. washwashed with deionized water three times
5. dry with materialdried over sodium carbonate
6. customThe solvent was removed on a Rotavapor
7. distillationVacuum distillation of the residue in the presence of the inhibitor