FORM-2
THE PATENTS ACT, 1970
(39 OF 1970)
PROVISIONAL SPECIFICATION
(SEE SECTION 10)
Title of invention: A PROCESS FOR THE PREPERATION OF 3'3 DICHLOROBENZEDINE HYDROCHLORIDE
Name and address of applicant:
SAJJAN INDIA LIMITED Matulya Centre, #2 Ground floor,
Senapati Bapat Marg, Lower Parel,
Mumbai - 400 013, Maharashtra, India.
Following specification particularly describes the nature of invention and the manner, in which it is to be performed.

PROCESS FOR THE PREPERATION OF 3'3 DICHLOROBENZEDINE
HYDROCHLORIDE
Field of Invention
The present invention relates to the process for the preparation of 3'3 Dichlorobenzedine hydrochloride and more particularly by the elimination of sulphuric acid, salt and water.
Prior Art
The preparation of 2,2 - DICHLOROHYDRAZOBENZEDINE is done by hydrogenation and/or catalytic reduction of 2,2 - Dichloroazoxybenzene which is well known commercial process.
The use of such process has several disadvantages. For instance 2,2HYD is in toluene and when mixed with it will go mixed into 60% to 62% Sulphuric Acid. This process takes 25 to 30 hrs under 25°C. This is called rearrangement reaction. When the entire HBT will be mixed with 60% Sulphuric acid will heat upto 52°C to 57°C and thereafter TLC ( Thin Layer Chromatography ) will be checked in toluene to reveal if 2,2 HYD appears or not. When TLC okay, then water is add water to it at 55°C. Subsequent to the addition of water will heat the mass upto 88°C to 93°C. At this temperature, the entire mass in the reactor will be converted into two layers. The top layer will be that of toluene while the lower layer would be that of the clear liquid solution consisting of sulphuric acid, water and 2,2 HYD to give 3,3 Dichlorobenzidine sulphate solution. The two layers are then separated and toluene is removed by distillation for reuse. There is loss of quantity of toluene and the waste effluent is removed in to the environment.
The lower layer is then heated to reach 88°C to 93°C so that the solution of 3,3

Dichlorbenzidine Sulphate will not be solidified. At the same temperature, some quantity of charcoal is added to remove impurities. On getting a clear homogenous liquid solution the charcoal is filtered out from the mass. After clarification of charcoal the temperature of the sulphate solution will continue to be maintained between 88°C to 93 °C.
In a new vessel a solution consisting of water having 25% of salt therein. The salt solution is also heated to 60°C to 70°C. The salt solution is added to the sulphate solution at 90°C. To this solution, further 30% HCL is added. This process is known as isolation. After charging of the HCL the cooling of entire mass will be started. The solution will be cooled to temperatures between 35°C to 40°C, when filter loss is checked. If filter loss is less than 1.5% of 3,3 Dichlorobenzidine Hydrochloride entire mass will be filtered through a nutsche. The cake on the filter is removed and made to dry to form 3,3 Dichlorobenzidine Hydrochloride. The filtered liquid solution is then put into effluent treatment plant for neutralization and reduction of COD and BOD as required by Pollution Control norms and incineration at temperatures of more than 900°C.
BRIEF SUMMARY OF THE INVENTION
The above and other objects of this invention are achieved by taking 2,2 -Dichloroazoxybenzene which is charged with any organic solvent and the temrature is either increased or decreased depending on the type of organic solvent being used. Agitation continues until the contents thereof becomes a homogenous solution which may or may not be clear. In the event the solution so formed is not clear then the same may be given carbon treatment or may be clarified or filtered by any of the known processes until the solution is clear. Once the solution is clear the temperature is lowered to a desired temperature and Hydrochloride gas or liquid is introduced while keeping the desired temperature constant. The Thin Layer Chromatograph (TLC) is

checked at regular intervals to confirm the presence of 2'2 Dichlorohydrazobenzene. When the checking results in showing that the presence of 2'2 Dichlorohydrazobenzene is nil, then the solution in the MS glass line jacketed vessel 3'3 Dicholorbenzedine hydrochloride.
DETAILED DESCRIPTION OF THE INVENTION
A MS glass line jacketed vessel is taken having an agitator fixed to it, in which 2'2 Dichlorohydrazobenzene either in solid or liquid form is introduced into the MS glass line jacketed vessel. To the 2'2 Dichlorohydrazobenzene in the MS glass lime jacketed vessel any organic solvent is charged which includes but is not limited to Methyl Ethyl Ketone (MEK), Toluene, Xylene, Acetone, Ethylene Dichloride (EDC), Methylenedichloride, Monochlorobenzene (MCB), Benzene. Agitation is commenced keeping the temperature of the contents of the MS jacketed glass line at room temperature generally but depending on the solvent being used the temperature may vary from 5°C to 100°C and the two ingredients will be constantly agitated to form a solution. The solution may or may not be clear on account of the impurities being present, hence the same be cleared by using the process of carbon treatment, clarification or filtration (using silicon oxide/silicon dioxide), thus the solution becomes clear/clarified. The temperature of the clear solution is lowered by cooling the MS glass line jacketed vessel and when the temperature of the MS jacketed glass line vessel is reached between 5°C to 50°C the same is kept constant and Hydro Chloride (HCL) is introduced which may be gaseous or liquid in nature. However gaseous or dilute HCL is preferred. On charging the solution with HCL isolation shall take place and thereafter the Thin Layer Chroma to graph (TLC) is checked. To confirm the presence of 2'2 Dichlorohydrazobenzene. When the checking results in showing that the presence of 2'2 Dichlorohydrazobenzene is nil then the remaining solution in the MS glass line jacketed vessel 3'3 Dicholorbenzedine hydrochloride.

DIAGRAM


The typical example given below to describe the invention do not limit compositional ranges covered under the ambit and scope of the present invention only.
EXAMPLE
A round bottom flask is taken in which lOOgms of 2'2 Dichlorohydrazobenzene is put after which organic solvent such as (200 ml of Toluene, 200 ml Xylene, 500 ml of Acetone, 500 ml MEK, 300 ml MCB, 300 ml EDC, 300 ml MDC) are added and the temperature is raised to be maintained between 40°C to 50°C which causes a clear solution to be prepared. To the solution in the event of impurities carbon treatment or clarification is done for removing the impurities. The reaction mass is constantly stirred and clarification is done in order to separate from the solution the organic layer. After the separation of the organic layer a further charge of 300 ml of Acetone

or 300 ml of Acetone along with 25ml of Acetic Acid or 300 ml of Acetone along with 15 ml of Sulphuric Acid or 300 ml of Petroleum Ether or 400 ml Methyl Ethyl Ketone and then 300 ml dilute HCL solution will be added but when the reaction is commenced with Methyl Ethyl Ketone is added then no further charge is required as stated herein. Pursuant to the clarification and charging as stated herein, the temperature is lowered maintained between 25°C to 30°C and 300 ml of HCL solution is added while the temperature is kept constant at 25C for 20 to 40 minutes. Thereafter the temperature is again raised to 30°C to 40°C and maintained for 3hrs to 5hrs and then the same is washed with either Acetone or Methyl Ethyl Ketone and then the reaction
mass sucked dry to yield gms/ml off 3'3Dichlorobenzedine
hydrochloride.
Variations
Yield is to % based on the use of Acetone or Methyl Ethyl Ketone
This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein; rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.

We claim,
1. A process for preparing 3,3 DichloroBenzedine Hydrochloride
comprising, Mixing 2,2 Dichloroazyxobenzene with organic solvent,
preferably acetone, Toulene in stainless steel (SS) jacketed reactor with
agitator, Raney Nickel is added to the reaction mass as a catalyst at
temperature between 40° C to 45°C; heating the same until the reaction mass
turns into a clear solution, on achieving the clear solution added carbon and
continue agitation, the continued agitation of the reaction liquid is introduced
into a RBF and allowed to settle until liquid will separate introducing
hydrogen gas to said reactor still completion of hydrogenation reaction;
filtering slurry of step (d) to separate Raney Nickel Catalyst; treating the
reaction mass of step (e) with carbon; filtering the reaction mass of step (f) to
remove the carbon from reaction mixture; transferring the reaction mass of
step (g) to MS glass line reactor, treating the reaction mass of step with
anhydrous HCL gas/liquid at temperature between OC to 55C; Filtering
precipitated slurry of step (i) and filtering washing and drying the leftover
cake to obtain 3,3 Dichloro Benzedine hydrochloride.
2. A process for preparing 3,3 DichloroBenzedine Hydrochloride such as
here in described with reference to an accompanying drawings