Reference of 5332-06-9, The chemical industry reduces the impact on the environment during synthesis 5332-06-9, name is 4-Bromobutanenitrile, I believe this compound will play a more active role in future production and life.
Piperidine (3 equiv.) and toluene (5.5 volumes based on 4-bromobutanenitrile weight) were mixed and heated to 55-60 C. To this mixture, 4-bromobutanenitrile (1 equiv.) was added slowly while keeping temperature below 80 C. Note the addition is exothermic and the exotherm is addition-controlled. A white solid was observed to crystallize during the addition (piperidine hydrobromide). After complete addition, the reaction was stirred at 55-60 C. for an additional 1 hour. Progress of the reaction was monitored by 1H NMR in CDCl3 by sampling from the slurry, filtering, and evaporating solvent. After reaction is finished, the mixture was cooled to 10-20 C. and stirred for 1 hour. Solids were removed by filtration, and the cake washed with toluene (2×1.5 volumes based on 4-bromobutanenitrile weight). The combined filtrates were evaporated under vacuum (15-50 mmHg) at 40-50 C. until 120-200% of the theoretical weight was obtained. The solution was again filtered to remove remaining piperidine hydrobromide solids. The filtrate was then further evaporated under vacuum (15-50 mmHg) at 40-50 C. until no more solvent distilled. 1H NMR in CDCl3 was done to quantify residual amount of toluene for correction in next step and to verify that there was no residual piperidine present.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 4-Bromobutanenitrile, other downstream synthetic routes, hurry up and to see.