STANDARD LABARATORY PROCESS

ABDT stage : 3

Phthalimide to potassium Phthalimide

Raw material

S.No Material Name Unit Quantity Remarks

01 Phthalimide ( Lot -1 ) g 75.00
02 KOH ( Lot-2 )) g 28.5
03 Methanol Ml 2130
04 Acetone (lot-1 ) Ml 75.00
05 Pthalimide g 75.00
06 KOH ( Lot-2 ) g 28.5
07 Acetone ( Lot-2) Ml 75.00

Laboratory process

S.No Operation Observation Remarks

01 Charge 1.9 L Methanol

02 Added Phthalimide ( Lot-1 ( 75.00 g

03 Heated the reaction mass to 60*C and

04 Maintain for 1.0 hr at 60*C Clear solution

05 Cool the reaction mass to 50*C and added Precipitate

KOH 28.5 g dissolved in 115 ml of methanol formed slowly
) ( pre cold to 20*C ) at 45 to 52*C
06 Cool the reaction mass to 20*C and maintain Solid formation
for 1.0 hrs at 15 to 20*C increases
07 Filter the solid and wash with 0.075 L ) of Free flowing Keep the
methanol solid filterate for
lot-2
reaction
08 Wash the solid with 75 ml of acetone Free flowing
solid
09 Unload and dry the product under vaccum till
to get M.C less than 0.5 % w/w ( product Lot-1
)
S.No Operation Observation Remarks

10 Charge the filterate methanol from operation

no : 7 and add (Lot-2 ) Phthalimide ( 0.075
Kg ) into the reactor
11 Heated the reaction mass to 60*C and maintain Clear solution
for 1.0 hrs
12 Cool the reaction mass to 50*C and added Precipitate
KOH 28.5 g dissolved in 115 ml of methanol formed slowly
) ( pre cold to 20*C ) at 45 to 52*C
13 Cool the reaction mass to 20*C and maintain Solid formation
for 1.0 hrs at 15 to 20*C increases
14 Wash the solid with acetone Free flowing
solid
15 Dry the solid till to get LOD less than 0.5 %
w/w ( Product Lot-2 )
16 Blend dried Lot-1 and lot-2

17 Distill our the filterate methanol at 45 to 50*C

under vaccum and take third crop

Out put : 120 g

Analysis :

Description : offwhite to sligh greenish cloured

LOD : NMT 0.5 % w/w
Identification by NMR
Suphated ash content : 45 to 48% w/w

Prepared by Checked by Approved by

k.vijay benadict raj Jai ganesh n.natarajan