反应详情

温度

150 °C

The autoclave is closed and the reaction mass is heated to 150°C (over a period of 50 minutes). The reaction mass is then maintained at a temperature of between 135°-160°C and at a pressure of 20 up to 60 psig for a period of 3 hours. At the end of this 3-hour period, the autoclave is opened and the reaction mass is cooled to room temperature. 12.6 g of sodium bicarbonate is then added to the reaction mass in order to neutralize the propionic acid. 30 g of Primol (see Note 1) and 0.1 g of Ionol (see Note 2 ) are added and the resulting reaction product is fractionally distilled at atmospheric pressure to a pot temperature of 129°C. A mixture of ethanol and ethyl propionate is distilled over. Vacuum is then applied to the distillation column and the resultant product, ethyl-2-methyl-3,4-pentadienoate is distilled at a vapor temperature of 65°-69°C at a pressure of 24-33 mm Hg as fractions 5-10 of the following fractions:

1. customThe autoclave is closed
2. temperatureThe reaction mass is then maintained at a temperature of between 135°-160°C and at a pressure of 20 up to 60 psig for a period of 3 hours
3. customAt the end of this 3-hour period
4. temperaturethe reaction mass is cooled to room temperature
5. customthe resulting reaction product
6. distillationis fractionally distilled at atmospheric pressure to a pot temperature of 129°C
7. additionA mixture of ethanol and ethyl propionate
8. distillationis distilled over
9. distillationVacuum is then applied to the distillation column
10. distillationthe resultant product, ethyl-2-methyl-3,4-pentadienoate is distilled at a vapor temperature of 65°-69°C at a pressure of 24-33 mm Hg as fractions 5-10 of the following fractions