Laboratory Experiments of B.Sc. II Sem BT/FS/CBZ - Experiment: 2

 

Laboratory Experiments of B.Sc. II Sem BT/FS/CBZ

 

Dr. Navdeep Sharma
Institute of Sciences
SAGE University, Indore (M.P.)

 

Experiment 2

Objective: Synthesis of Oxime from a Carbonyl Compound

                                               

Objective:

To synthesize an oxime from an aldehyde or ketone using hydroxylamine hydrochloride (NH₂OH·HCl).

Materials Required:

• Carbonyl compound (aldehyde or ketone) – 2 mL
• Hydroxylamine hydrochloride (NH₂OH·HCl) – 2 g
• Sodium hydroxide (NaOH) solution (10%) – 5 mL
• Ethanol (or methanol) – 10 mL
• Distilled water – 10 mL
• Ice bath
• Beaker (50 mL or 100 mL)
• Glass rod
• Filter paper & funnel
• Watch glass

Stepwise Procedure:

1. Preparation of Hydroxylamine Solution:
• Dissolve 2 g of hydroxylamine hydrochloride in 10 mL of distilled water in a beaker.
• Add 5 mL of 10% sodium hydroxide solution to free hydroxylamine (NH₂OH).
2. Reaction with Carbonyl Compound:
• Take 2 mL of the aldehyde or ketone in another beaker.
• Add 10 mL of ethanol (or methanol) to dissolve the compound.
• Slowly add the hydroxylamine solution to the carbonyl solution while stirring.
3. Mixing and Heating:
• Stir the mixture well and heat gently (40–50°C) for 10–15 minutes to complete the reaction.
4. Precipitation and Cooling:
• Allow the reaction mixture to cool to room temperature and then place it in an ice bath to promote crystal formation.
5. Filtration and Washing:
• Filter the solid oxime product using filter paper.
• Wash the precipitate with cold distilled water to remove impurities.
6. Drying and Storage:
• Transfer the oxime to a watch glass and let it air-dry or dry it in a desiccator.

Observation:

• The oxime product will be a solid crystalline compound with a melting point characteristic of the specific carbonyl compound used.