反应详情

温度

25 °C

A dry 1 liter 3-neck round-bottom flask was charged with a magnetic stir bar and equipped with three septa. A nitrogen purge was introduced through a needle with output, also via a needle, to an oil bubbler. A thermocouple lead was placed through a side neck septa. Excess zinc (150 grams, ‘dust’ was found more conducive to stirring) was added to the flask. By syringe, 2,4-dimethyl-1,3-pentadiene (25 grams, 0.26 mol) was added to the flask. By cannula, ruthenium trichloride hydrate (6.0 grams, 0.023 mol based on 3 hydrate equivalents) was added as a methanol (250 milliliters) solution in spurts of about 10 milliliters over 45 minutes. The mixture was stirred for 30 minutes at 25° C. after the addition was complete, then, upon equipping a condenser, the contents were brought to gentle reflux. Stirring was continued for 2 hours. The mixture was cooled to 25° C., followed by the addition of freshly distilled 1,3-dimethylcyclopentadiene (2.2 grams, 0.023 mol) by syringe over 20 minutes. Stirring was continued at 25° C. for 20 additional minutes, followed by gentle reflux for 2 hours.

1. additionA dry 1 liter 3-neck round-bottom flask was charged with a magnetic stir bar
2. customequipped with three septa
3. customA nitrogen purge
4. additionwas introduced through a needle with output, also via a needle, to an oil bubbler
5. customA thermocouple lead was placed through a side neck
6. additionwas added to the flask
7. stirringThe mixture was stirred for 30 minutes at 25° C.
8. additionafter the addition
9. stirringStirring
10. stirringStirring
11. customwas continued at 25° C. for 20 additional minutes
12. temperatureby gentle reflux for 2 hours