Synthesis Of 1-Bromobutane Lab Report
In this experiment, we used simple distillation and extraction to do synthesis of 1-bromobutane. The experiment was carried out by mixing 13.3 g of sodium bromide, 15 mL of water and 10 mL of n-butyl alcohol in a 100 mL round bottom flask. We cooled the mixture and added 11.5 mL of concentrated sulfuric acid. Then the mixture was heated at reflux with a short condenser for 45 minutes and then we drained out the condenser. We removed the condenser and distillation head was set up to set up the condenser for simple distillation. We distilled the mixture until no more water soluble droplets came over. We poured the distillate into a separatory funnel and added 10 mL of water which formed 2 layers an organic and aqueous layer. The organic layer
with 1-bromobutane was poured into a flask and back into a clean separatory funnel and cooled 10 mL of concentrated sulfuric acid was added to the funnel and we waited for 5 minutes for complete separation of the layers. We poured the aqueous bottom layer in the flask and waited for another 5 minutes to completely separate the layers again and was separated again. We washed the organic 1-bromobutane with 10 mL of 3M sodium hydroxide to remove the traces of acid, and separated the 2 layers again. We dried the cloudy 1-bromobutane by adding anhydrous sodium sulfate and calcium chloride pellets until the liquid cleared out. After a while we decanted the liquid into a flask and distilled again using simple distillation.
Distill which is the final product 1-bromobutane was collected in the pre-weighed sample vial in between the temperature range of 94.8 °C – 95.5 °C. Based on the boiling range of 94.8 °C - 95.5 °C we assume that the final product is pure because the boiling range of final product is lower than the boiling range of n-butyl alcohol, sulfuric acid and water. Final product appeared colorless clear liquid and actual yield and percent yield was calculated. Actual yield was 5.425 g and % yield was 36.3%. During extraction and simple distillation, we might have not recovered all the product which might have affected the % yield of the final product.
with 1-bromobutane was poured into a flask and back into a clean separatory funnel and cooled 10 mL of concentrated sulfuric acid was added to the funnel and we waited for 5 minutes for complete separation of the layers. We poured the aqueous bottom layer in the flask and waited for another 5 minutes to completely separate the layers again and was separated again. We washed the organic 1-bromobutane with 10 mL of 3M sodium hydroxide to remove the traces of acid, and separated the 2 layers again. We dried the cloudy 1-bromobutane by adding anhydrous sodium sulfate and calcium chloride pellets until the liquid cleared out. After a while we decanted the liquid into a flask and distilled again using simple distillation.
Distill which is the final product 1-bromobutane was collected in the pre-weighed sample vial in between the temperature range of 94.8 °C – 95.5 °C. Based on the boiling range of 94.8 °C - 95.5 °C we assume that the final product is pure because the boiling range of final product is lower than the boiling range of n-butyl alcohol, sulfuric acid and water. Final product appeared colorless clear liquid and actual yield and percent yield was calculated. Actual yield was 5.425 g and % yield was 36.3%. During extraction and simple distillation, we might have not recovered all the product which might have affected the % yield of the final product.