Process for the preparation of malathion and its intermediate
AssigneeSuven Life Sciences Limited
InventorsVeera Reddy Arava, Vaishali Nadkarni, Venkateswarlu Jasti
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Abstract
The present invention relates to the improved process for the preparation of highly pure form of S-[1,2-(dicarbethoxy)-ethyl]O,O-dimethyl phosphorodithioate having formula (I). The compound of formula (I) has adopted name “Malathion”. The present invention also relates to the novel process of preparing intermediate O,O-dimethyldithiophosphoric acid of formula (II), which is useful in the preparation of Malathion.
Claims15
A process for the preparation of Malathion of formula (I),
- which comprises the steps of:
- i) adding methanol to phosphorous sulfide in organic solvent at 25-50° C. for a period of 1.5-2 hours;
- ii) stirring the above suspension for a period of 5-6 hours at 50-55° C.;
- iii) expelling the H2S gas with nitrogen, after cooling the above suspension to 25-28° C.;
- iv) filtering the above suspension to remove insoluble impurities to obtain crude O,O-DMDTPA;
- v) the crude O,O-DMDTPA is subjected to dissolution in suitable solvent and ammonia gas is purged to precipitate pure O,O-DMDTPA.NH3 salt;
- vi) the above obtain O,O-DMDTPA.NH3 salt is subjected to neutralization with concentrated sulphuric acid to get O,O-DMDTPA;
- vii) the O,O-DMDTPA obtained in the above step is once again purified through ammonia salt formation and neutralization method as mentioned in above steps v) and vi) to get chromatographically pure O,O-DMDTPA of the formula II
- viii) adding the above obtain pure O,O-DMDTPA to diethyl maleate at low temperature of −30 to −25° C. in four lots, each at regular interval of 20 minutes;
- ix) maintaining the above reaction mass at temperature of −30 to −25° C. for a period of 4 hours;
- x) water washing the above mass to remove O,O-DMDTPA;
- xi) treating the above obtain crude Malathion with a sulfur reagent at 5 to 10° C. for a period of 13 hours;
- xii) crystallizing the above obtained Malathion from methanol at low temperature and
- xiii) drying the above obtain mass with anhydrous sodium sulphate in isopropanol to obtain Malathion of formula (I).
A process for the preparation of intermediate O,O-dimethyldithiophosphoric acid of formula (II)
- for use in the preparation of Malathion, which comprises the steps of:
- i) adding methanol to phosphorous sulfide in organic solvent at 25-50° C. for a period of 1.5-2 hours;
- ii) stirring the above suspension for a period of 5-6 hours at 50-55° C.;
- iii) expelling the H2S gas with nitrogen, after cooling the above suspension to 25-28° C.;
- iv) filtering the above suspension to remove insoluble impurities to obtain crude O,O-DMDTPA;
- v) the crude O,O-DMDTPA is subjected to dissolution in ethyl acetate and ammonia gas is purged to precipitate the pure O,O-DMDTPA.NH3 salt;
- vi) the above obtain O,O-DMDTPA.NH3 salt is subjected to neutralization with concentrated sulphuric acid to get O,O-DMDTPA and vii) the O,O-DMDTPA obtained in the above step is once again purified through ammonia salt formation and neutralization method as mentioned in above steps v) and vi) to get chromatographically pure product.
Dependencies are inferred from the claim text.