Conversion of phenol to p-nitrosophenol

CARE SHOULD BE TAKEN WHILE DOING THIS EXPERIMENT
 In my M.Sc project I got the opportunity to do the synthesis of paracetamol from phenol  at Kerala State Drugs & pharmaceuticals Ltd in Kerala State.This experiment is the first stage in the conversion of phenol  to paracetamol.

AIM:

To convert phenol to p-nitrosophenol.

RAW  MATERIALS:

• Phenol 9.41gm
• distilled water  10ml
• 20ml 50 % con sulphuric acid
• Ice
• Sodium nitrite solution( 6.9gm  dissolved in 10ml distilled water)
• Chilled water

APPARATUS:

• 250ml beaker
• Vessel filled with water( for cooling purpose)
• Thermometer
• Centrifuge
• glass rod

PROCEDURE:

• In a beaker approximately 9.41g phenol & 10ml water  is taken.
• The contents in the beaker are cooled to +9 degree celsius by placing it in a vessel filled with water.
• The temperature is noted with the help of a thermometer.
• When the temperature is +9 degree celsius add 20ml 50% con sulphuric acid slowly with the help of a glass rod & ice is charged to it to bring down the temperature to +2 degree celsius.
• When the temperature is +2 degree celsius, sodium nitrite solution is slowly added to the beaker.
• On complete addition, the beaker is taken out from the vessel & the contents are kept stirred for 1 hour to complete the formation of nitroso product.
• This is then centrifuged  & washed with chilled water to remove sulphates.
• The p-nitrosophenol obtained is kept ready for the next reaction.

I took 2 hours  for completing the reaction.

STUDENTS SHOULD PERFORM THIS EXPERIMENT ONLY WITH THE HELP OF A TEACHER.