Antibumping granules

In a single-necked round-bottomed flask (2 L), prepare a solution of diethyl malonate (16 g, 0.1 mol) in ethanol (1.0 L), and add 1,5,9-triazanonane (13,1 g, 0.1 mol) and a few antibumping granules. Attach a reflux condenser surmounted by a drying tube and boil the solution under reflux for 5 d. Remove the solvent on a rotary evaporator (care use an anti-splash device to help avoid bumping ) and dissolve the residue in the minimum volume of dichloromethane-methanol (90 10 c. 10 mL). 

If the mantle is not equipped with a stirrer, remember to add antibumping granules (p. 31) to the liquid. 

Add the liquid to be distilled to the distillation flask using a stemmed funnel, together with antibumping granules or boiling stick or a magnetic flea . The flask should not be more than 50% full. Reclamp the flask in position. 

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