Carbon Tetrachloride → 9,9-Dichloro-9H-fluorene

Participants

Reaction Steps

To the reactor which has been purged with nitrogen is charged a volume of carbon tetrachloride (400 mL) such that its level just comes to the bottom of the sixth stage. NaOH solution (the same solution used in the previous run (Example 49), Part A), 25 percent by weight, 6.14 moles, 245.6 g dry weight, 983 g solution weight, 774.0 mL) is then charged to the reactor, and fills all six of the stirred zones. The stirrer is started and its speed adjusted to 1500 rpm. Fluorene (0.185 moles, 30.75 g) dissolved in carbon tetrachloride (2.24 moles, 344.8 g, 225.35 mL) is fed into the catalyst saturator containing the catalyst solution using a metering pump at a rate of 5.5 mL/min. The product solution is collected at the overflow and washed and dried as in Part A. The total product solution collected in this fashion amounts to 1056 g which is evaporated to dryness on a rotary evaporator leaving 42.66 g of very light yellow crystals, 9,9-dichlorofluorene (98.1 percent of the theoretical yield of 43.49 g).

Provenance & Evidence