Реакция #302873
ord-669cd56648894d7da16df5c19ad75e04
Уравнение реакции
N,N-dimethylammonium iodide
2,2-dimethyl-5-phenyl-[1,3]dioxane-4,6-dione
→
2-phenyl acrylic acid methyl ester
Выход 102.7%
Реагенты
Нет
Растворители
Условия реакции
Подробные условия
See reaction.notes.procedure_details.
Обработка
- 1workup.WAITto continue over night at 65° C
- 2Другоеthe solvent was removed under reduced pressure
- 3workup.ADDITIONThe residue was treated with diethyl ether
- 4Экстракцияextracted with a satured NaHCO3 solution and brine
- 5Сушкаdried over MgSO4
- 6ДругоеThe solvent was removed under reduced pressure
Методика
A solution of 25 g (135.1 mmol) N,N-dimethylammonium iodide and 11.91 g (54.1 mmol) 2,2-dimethyl-5-phenyl-[1,3]dioxane-4,6-dione in 585 ml abs. methanol was heated to 65° C. and the reaction was allowed to continue over night at 65° C. The reaction mixture was allowed to cool down to room temperature and the solvent was removed under reduced pressure. The residue was treated with diethyl ether, extracted with a satured NaHCO3 solution and brine and dried over MgSO4. The solvent was removed under reduced pressure and 9.01 g (quant.) of 2-phenyl acrylic acid methyl ester was isolated as a colourless oil. The compound was used without further purification.