反应详情

400 g of 1,2-dimethoxy ethane were introduced into a 1 liter glass flask equipped with a stirrer and a thermometer and admixed with 69 g of gaseous hydrogen chloride. 184.1 g of 1-vinyl-2,2-dicarbomethoxy cyclopropane (93.7% pure, 0.937 mol) and 0.65 g of aluminum chloride were then added to the contents, and the mixture was stirred. The temperature of the mixture rose to 40° C. The reaction was allowed to go to completion by letting the mixture stand overnight. After filtering off a slight turbidity, the reaction mixture was distilled in a 70 cm column. After collecting the 1,2-dimethoxy ethane which distilled over first and became available for reuse as a solvent in subsequent batches, the target product distilled over in pure form at 87° C./0.8 mbar.

1. customequipped with a stirrer
2. customrose to 40° C
3. filtrationAfter filtering off a slight turbidity
4. distillationthe reaction mixture was distilled in a 70 cm column
5. customAfter collecting the 1,2-dimethoxy ethane which
6. distillationdistilled over first and
7. distillationthe target product distilled over in pure form at 87° C./0.8 mbar