16.9 g of 75°C hot 3′-chloropropiophenone is added to a beaker and it is brominated with 18 g of bromine with stirring. The bromine should be added at a constant rate of 1 drop per second, after the addition, the solution is heated at 75°C for 3h. The solution is poured into a reflux apparatus with 29 g of t-butylamine, the solution is refluxed for 5.5h, the excessive t-butylamine is distilled off from the solution below at 90°C. The product is poured into 100 mL of water and it is then extracted twice with 25 mL of DCM, the DCM is evaporated off and the product is dried over anhydrous magnesium sulfate.
(The equipment and procedures are different below because of the batch size.)
Addition of the bromine
Isolation of the compound
Addition of the t-BA
Drying the pure product