反应详情

Into a 100 ml long neck round bottom flask with a vacuum adapter is placed about 2 g of 3 A molecular sieves. The flask is connected to a vacuum line and placed under reduced pressure of about 0.02 mm of Hg. It is then heated, causing gas (air) to evolve from the sieves. Heating is continued until gas evolution ceases. Then the flask is allowed to cool to room temperature and the vacuum adapter is removed. Solvent in the form of 50 ml of carbon tetrachloride is then added to the flask along with 25 mmol of 3-methyl-3-pentanol and 25 mmol of methacryloyl chloride. A magnetic stirring bar is added to the contents of the flask and a condenser with a drying tube is attached to the neck of the flask. Then the flask and its contents are placed in a hot water bath and heated for 185 hours while being subjected to magnetic stirring. The contents of the flask are then cooled and filtered through a celite pad, filtered through a 20 cm Al2O3 column, the column washed with 100 ml of CH2Cl2 and the solvents are then evaporated under reduced pressure. The resulting product is pure monomeric 3-methyl-3-pentyl methacrylate ester.

1. customInto a 100 ml long neck round bottom flask with a vacuum adapter is placed
2. temperatureIt is then heated
3. temperatureHeating
4. customthe vacuum adapter is removed
5. additionA magnetic stirring bar is added to the contents of the flask and a condenser with a drying tube
6. customThen the flask and its contents are placed in a hot water bath
7. temperatureheated for 185 hours
8. temperatureThe contents of the flask are then cooled
9. filtrationfiltered through a celite pad
10. filtrationfiltered through a 20 cm Al2O3 column
11. washthe column washed with 100 ml of CH2Cl2
12. customthe solvents are then evaporated under reduced pressure