Question

propose a method (technique) to purify and isolate the product, 1-bromobutane, only from the crude product mixture. provide detailed procedure for the method you choose for full credit.

Answer 1

To purify and isolate 1-bromobutane from the crude mixture, you can use solvent extraction, reflux, and column chromatography. These steps should yield the product with a 58% yield, and it can be characterized by spectroscopic techniques.

Step-by-step explanation:

To purify and isolate the product, 1-bromobutane, from the crude mixture, you can use a combination of solvent extraction, reflux, and column chromatography.

1. First, dissolve the crude product in n-BuOH (3 mL).
2. Add 5-amino-4,6-dichloropyrimidine (140.1 mg, 0.86 mmol) and i-Pr₂NEt (298 µL, 1.71 mmol) to the mixture.
3. Keep the mixture under reflux overnight.
4. Remove the solvents under reduced pressure.
5. Purify the residue by using silica gel column chromatography with a mixture of chloroform-methanol (19:1) as the eluent.

This method should yield 1-bromobutane with a 58% yield. The product can be characterized by various spectroscopic techniques like ¹H-NMR, ¹³C NMR, IR, EI-MS, and HRMS.