Dividol ,Zambon ,Italy ,1974
10 g (0.0278 mol) of 1-(o-chloro)-benzyl-2-di-sec-butylaminoacetyl-pyrrole
and 300 ml of anhydrous diethyl ether are placed in a 500 ml four-necked
flask with a mercury-sealed stirrer, a thermometer, a dropping funnel and a
reflux condenser topped with a tube containing anhydrous calcium chloride.
The solution is stirred and a mixture of 1g (0.0264 mol) of lithium aluminum
hydride in 20 ml of diethyl ether is added slowly through the dropping funnel
at such a rate that the solvent refluxes gently without external heating. When
the addition is complete and the initial reaction subsides, the mixture is
stirred and heated at gentle reflux for two hours.
The mixture is cooled and the excess of lithium aluminum hydride is
decomposed with cracked ice. The water layer is separated and washed with
diethyl ether. The combined ether extracts are dried over anhydrous
magnesium sulfate and the solvent is removed by distillation under reduced
pressure. Yield, 8.8 g; boiling point, 160°C to 165°C/0.1 mm Hg.
