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Standard Operating Procedure For Bispyribac Sodium Manufacturing
Standard Operating Procedure For Bispyribac Sodium Manufacturing
BISPYRIBAC
SODIUM
1. PURPOSE:
To Establish the documented procedure for manufacturing of Bispyribac sodium as per the
specified process.
2. SCOPE:
This SOP is applicable for the manufacturing of Bispyribac sodium as per the specified process.
3. RESPONSIBILITY:
Designation Responsibility
All the employees To follow the procedure of training.
In-Charge-Production Production Incharge to ensure the proper execution
Head Production Overall responsible for implementation of SOP.
4. DEFINITION OF TERMS
May cause respiratory contact lenses, if present and easy to protective gloves,
irritation. do. Continue rinsing. e.g., PVC
If breathed in, move person into Wear safety footwear
fresh air. If not breathing, give
artificial respiration. Consult a
physician.
In case of skin contact: Wash off
with soap and plenty of water.
Consult a physician.
In case of eye contact: Rinse
thoroughly with plenty of water for
at least 15 minutes and consult a
physician.
If swallowed: Never give anything
by mouth to an unconscious person.
Rinse mouth with water. Consult a
physician
2-Methylsulfonyl-4,6- Not a hazardous Avoid dust formation. Avoid Safety glasses with
dimethoxypyrimidine substance or mixture breathing vapors, mist, or gas. side shields.
according to Wear chemical
Regulation (EC) No. protective gloves,
1272/2008 e.g., PVC
Wear safety footwear
Dimethylformamide Flammable liquid and Avoid breathing Wear personal
vapor dust/fume/gas/mist/vapors/spray protective
Causes serious eye Keep away from heat/sparks/open equipment/face
irritation flames/hot surfaces. - No smoking protection
May damage the Use only outdoors or in a well- Safety glasses with
unborn child ventilated area side shields.
Harmful in contact IF exposed or concerned: Get Wear chemical
with skin or if inhale medical attention/advice protective gloves,
IF INHALED: Remove victim to e.g., PVC
fresh air and keep at rest in a Wear safety footwear
position comfortable for breathing
Skin: Call a POISON CENTER or
doctor/physician if you feel unwell
OUTPUT QUANTITY
Sr. No. OUTPUT QUANTITY (KG) QUANTITY (LTR)
1 BISPYRIBAC SODIUM ~250 Kg ~170 Ltr
7. GENERAL CHECKPOINTS
Inspection of Equipment’s
I. Inspect the reactor and ensure that it is empty, leak proof and there is no residual mass of last batch
into the reactor.
I. Close the bottom valve of the reactor. In case of material is to receive in drums/bags, verify
the label of Raw material, quantity by weighing the quantity on calibrated weighing
balance.
II. Ensure that all the utilities and instruments are working properly.
8. OPERATING PROCEDURE
STEP-I: CARBAMATE INTERMEDIATE FORMATION
• Inspect the reactor and ensure that it is empty, leak proof and there is no residual mass of
last batch into the reactor.
• Ensure that all the utilities and instruments are working properly.
• Charge weighted quantity of DMF in SS reactor at ambient temperature and start the
utility circulation in condensers.
• Start the agitator and charge weighted quantity of Toluene in SS reactor at ambient
temperature.
• Charge weighted quantity of Dihydroxy benzoic acid under stirring followed by
potassium carbonate through manhole at ambient temperature.
• Stir the reaction mass for 10-15 minutes after RM charging.
*Note: Exothermicity of 3-5 °C may observe after potassium carbonate charging.
• Now gradually increase the temperature of reaction mixture upto 110-115°C by providing
steam circulation in reactor jacket.
• Once temperature is reached keep the reaction mixture under reflux for 3-4 Hrs. to
separate the water from azeotropic mixture.
• Cool the reaction upto 40°C by circulating cooling water in reactor jacket.
Action Prepared By Reviewed By Approved By
Name
• Now start the dosing of weighted quantity of 32% HCl from addition pot to reaction mass
at 30-35°C.
• Reaction mass temperature to be maintained by using cooling water circulation in reactor
jacket.
• Check the pH of reaction mass it should be around 2-2.5.
• Heat the reaction mass upto 50°C and maintain it for 1 Hr.
• Filter the reaction mass at same temperature through rubber coated filter. (As material is
acidic in nature)
• Wash the wet cake with weighted quantity of water and filter the wash ML.
• Unload the wet cake in polybag from filter for further process.
STEP-IV: DRYING
• Prepare Tray Dryer (SS Dryer) and check the utility circulation.
• Fill the Dryer trays with measured quantity of Bispyribac Sodium wet cake.
• After complete filling apply the heating in Dryer upto 70-80°C.
• Start the drying of Bispyribac Sodium at 70-80°C.
• Send the sample of material for M/C check. If M/C is less than 1% then apply cooling
upto 35-40°C and do the unloading of Bispyribac Sodium else continue the drying at 70-
80°C.
• Expected Dry Bispyribac Sodium = 250 Kg
*Note: Use Necessary PPE’s while manual unloading of dry Bispyribac Sodium.
• Properly Label the Dry Bispyribac Sodium bags.
• Keep the reaction & filtration system ready for next batch.