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11 Nov 2019
Part-II Synthesis & Spectroscopy Experiment 18. Synthesis of 1-Bromobutane Procedure: 7.5 g of 1-butanol was added to a solution of 10.3 g of sodium bromide in 10 mL of water. The solution was cooled in ice-water bath and 10 mL of concentrated sulfuric acid with swirling. The reaction mixture was refluxed gently for 45 minutes and simple distillation was performed rapidly until the distillation until the distillate is clear. The distillate was transferred to a separatory funnel and washed with 10 mL of water. The organic layer separated was washed with 0.2 M aqueous NaOH solution and then with 10 mL of saturated NaCl and dried over anhydrous sodium sulfate. The crude 1-bromobutane product was purified by simple distillation afforded 72% yield. 1. Write a balanced equation and the mechanisnm 2. What is the difference(s) between refluxing and distillation? 3. Discuss the purpose of a) washing the distillate with water b) washing the organic layer with i) 0.2 M aqueous NaO solution ii) saturated NaC 4. How many grams of 1-bromobutane was produced? 5. Discuss the 1H-NMR and IR spectroscopy of 1-Bromobutane and 1-butanol
Part-II Synthesis & Spectroscopy Experiment 18. Synthesis of 1-Bromobutane Procedure: 7.5 g of 1-butanol was added to a solution of 10.3 g of sodium bromide in 10 mL of water. The solution was cooled in ice-water bath and 10 mL of concentrated sulfuric acid with swirling. The reaction mixture was refluxed gently for 45 minutes and simple distillation was performed rapidly until the distillation until the distillate is clear. The distillate was transferred to a separatory funnel and washed with 10 mL of water. The organic layer separated was washed with 0.2 M aqueous NaOH solution and then with 10 mL of saturated NaCl and dried over anhydrous sodium sulfate. The crude 1-bromobutane product was purified by simple distillation afforded 72% yield. 1. Write a balanced equation and the mechanisnm 2. What is the difference(s) between refluxing and distillation? 3. Discuss the purpose of a) washing the distillate with water b) washing the organic layer with i) 0.2 M aqueous NaO solution ii) saturated NaC 4. How many grams of 1-bromobutane was produced? 5. Discuss the 1H-NMR and IR spectroscopy of 1-Bromobutane and 1-butanol
Hubert KochLv2
19 Oct 2019