AlMe 3 (2.0 M in toluene, 15.00 cm 3 , 30.00 mmol) was slowly added by syringe to a stirred solution of pyridine (3.00 cm 3 , 37.2 mmol) in toluene (20 cm 3 ) at room temperature. Subsequently, all volatiles were thoroughly removed under dynamic vacuum at room temperature to afford colorless crystals of the product (4.429 g, 97.7 %). The drying time had to be carefully controlled to avoid excessive product loss. The compound must be stored in gas-tight containers as it continuously resublimes to form large crystals on the container walls.