STEP 1: In a 100-ml
round-bottomed flask place 16.1 g (0.10 mol) of 3-bromocyclohexene, 38.7
g of dried, redistilled quinoline and a magnetic stirrer follower.
STEP 2: Attach to the
flask a Claisen still-head fitted with a thermometer and a condenser set for downward distillation.
STEP 3: Protect the apparatus from atmospheric moisture by a calcium chloride
guard-tube attached to the sidearm of the
receiver.
STEP 4: Support the reaction flask in an oil bath which rests on a magnetic
stirrer/hotplate, commence stirring rapidly and heat the oil bath to 160-170 °C.
STEP 5: The cyclohexadiene steadily distils as colourless liquid, b.p. 8082 °C, over a period of
about 30 minutes, yield 5.4 g (68%).
STEP 6: The product is 99 per cent pure by g.l.c.
analysis; use either a 2.7 m column of 10 per cent polyethyleneglycol adipate on Chromosorb W held at
60 °C with a flow rate of carrier gas of 40
ml/minute, tR 2.4 minutes, or, a 1.5 m
column of 10 per cent Silicone oil on Chromosorb W held at 6 °C with a
flow rate of carrier gas of 40 ml/minute, tR 1.5 minutes.
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